#########################################################################
# #
# THIS IS AN EXAMPLE OF A CIF REPORTING A SINGLE #
# STRUCTURE AND INCLUDING USER-DEFINABLE TEXT #
# SECTIONS #
# #
#########################################################################
data_global
loop_
_publ_body_element
_publ_body_title
_publ_body_contents
section .
;
?
;
section
;
Introduction
;
;\
INTRODUCTION TEXT HERE
;
section Experimental
;
?
;
subsection 'Synthesis and crystallization'
;
TEXT HERE
;
subsection Refinement
;
TEXT HERE
;
section 'Results and discussion'
;
TEXT HERE
;
#=============================================================
_audit_creation_date 'June 17, 2013'
_audit_creation_method 'from SHELXL-97'
_audit_update_record
;
;
#===================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name 'NAME'
_publ_contact_author_address
;
ADDRESS
;
_publ_contact_author_phone ?
_publ_contact_author_fax ?
_publ_contact_author_email ?
_publ_requested_journal 'Acta Crystallographica C'
_publ_requested_category FA
_publ_requested_coeditor_name ?
_publ_contact_letter
;
;
#=====================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_paper_doi ?
_journal_paper_category FA
_journal_coeditor_notes ?
_journal_techeditor_code ?
_iucr_compatibility_tag ACTA95
_journal_techeditor_notes ?
_journal_coden_ASTM ACSCGG
_journal_name_full 'Acta Crystallographica, Section C'
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#=====================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
TITLE
;
loop_
_publ_author_name
_publ_author_address
_publ_author_email
_publ_author_footnote
'NAME'
;
ADDRESS
;
? ?
#======================================================================
# 4. TEXT
_publ_section_synopsis
;
TEXT HERE
;
_publ_section_keywords
;
TEXT HERE
;
_publ_section_abstract
;
TEXT HERE
;
_publ_section_references
;
REFERENCES HERE
;
_publ_section_figure_captions
;
FIGURE CAPTIONS HERE
;
_publ_section_table_legends
;
TABLE CAPTIONS HERE
;
_publ_section_acknowledgements
;
ACKNOWLEDGEMENTS HERE
;
#=====================================================================
data_I
#=====================================================================
# 5. Chemical Data
_chemical_name_systematic
;\
(6R*,11R*)-5-Acetyl-11-ethyl-6,11-dihydro-5H-\
dibenzo[b,e]azepine-6-carboxylic acid
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C19 H19 N O3'
_chemical_formula_sum 'C19 H19 N O3'
_chemical_formula_weight 309.35
_chemical_compound_source 'synthesised by authors, see text'
_chemical_formula_iupac 'C19 H19 N O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21'
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 8.8053(3)
_cell_length_b 10.9821(4)
_cell_length_c 9.0080(6)
_cell_angle_alpha 90.00
_cell_angle_beta 118.510(3)
_cell_angle_gamma 90.00
_cell_volume 765.45(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 120(2)
_cell_measurement_reflns_used 1853
_cell_measurement_theta_min 3.20
_cell_measurement_theta_max 27.50
_exptl_crystal_description rod
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.342
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 328
_exptl_absorpt_coefficient_mu 0.091
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)'
_exptl_absorpt_correction_T_min 0.977
_exptl_absorpt_correction_T_max 0.991
_exptl_special_details
?
_diffrn_ambient_temperature 120(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method '\f and \w'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 13276
_diffrn_reflns_av_R_equivalents 0.0486
_diffrn_reflns_av_sigmaI/netI 0.0321
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_theta_min 3.71
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_reflns_number_total 1851
_reflns_number_gt 1638
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'COLLECT (Nonius, 1998)'
_computing_cell_refinement
'DIRAX/LSQ (Duisenberg et al., 2000)'
_computing_data_reduction
'EVALCCD (Duisenberg et al., 2003)'
_computing_structure_solution 'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
#=========================================================================
# 8. Refinement Data
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.1657P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_chemical_absolute_configuration unk
_refine_ls_number_reflns 1851
_refine_ls_number_parameters 210
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0455
_refine_ls_R_factor_gt 0.0360
_refine_ls_wR_factor_ref 0.0807
_refine_ls_wR_factor_gt 0.0772
_refine_ls_goodness_of_fit_ref 1.146
_refine_ls_restrained_S_all 1.146
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.209
_refine_diff_density_min -0.240
#=========================================================================
# 9. Atomic Coordinates and Displacement Parameters
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6424(3) 0.5942(2) 0.7939(3) 0.0186(5) Uani 1 1 d . . .
H1 H 0.6599 0.6154 0.9031 0.022 Uiso 1 1 calc R . .
C2 C 0.7828(3) 0.5595(2) 0.7731(3) 0.0211(5) Uani 1 1 d . . .
H2 H 0.8953 0.5589 0.8678 0.025 Uiso 1 1 calc R . .
C3 C 0.7604(3) 0.5255(2) 0.6149(3) 0.0202(5) Uani 1 1 d . . .
H3 H 0.8563 0.4993 0.6019 0.024 Uiso 1 1 calc R . .
C4 C 0.5955(3) 0.5306(2) 0.4757(3) 0.0166(5) Uani 1 1 d . . .
H4 H 0.5780 0.5079 0.3669 0.020 Uiso 1 1 calc R . .
C4a C 0.4576(3) 0.5687(2) 0.4973(3) 0.0142(5) Uani 1 1 d . . .
N5 N 0.2883(2) 0.58197(17) 0.3533(2) 0.0132(4) Uani 1 1 d . . .
C6 C 0.1469(3) 0.4966(2) 0.3244(3) 0.0128(4) Uani 1 1 d . . .
H6 H 0.0389 0.5461 0.2831 0.015 Uiso 1 1 calc R . .
C6a C 0.1714(3) 0.4295(2) 0.4842(3) 0.0145(5) Uani 1 1 d . . .
C7 C 0.1243(3) 0.3077(2) 0.4737(3) 0.0174(5) Uani 1 1 d . . .
H7 H 0.0884 0.2652 0.3704 0.021 Uiso 1 1 calc R . .
C8 C 0.1286(3) 0.2465(2) 0.6107(3) 0.0189(5) Uani 1 1 d . . .
H8 H 0.0977 0.1628 0.6008 0.023 Uiso 1 1 calc R . .
C9 C 0.1780(3) 0.3073(2) 0.7616(3) 0.0188(5) Uani 1 1 d . . .
H9 H 0.1759 0.2670 0.8540 0.023 Uiso 1 1 calc R . .
C10 C 0.2305(3) 0.4277(2) 0.7762(3) 0.0185(5) Uani 1 1 d . . .
H10 H 0.2674 0.4685 0.8808 0.022 Uiso 1 1 calc R . .
C10a C 0.2307(3) 0.4909(2) 0.6412(3) 0.0151(5) Uani 1 1 d . . .
C11 C 0.3097(3) 0.6185(2) 0.6677(3) 0.0150(5) Uani 1 1 d . . .
H11 H 0.2307 0.6694 0.5686 0.018 Uiso 1 1 calc R . .
C11a C 0.4763(3) 0.5982(2) 0.6566(3) 0.0145(5) Uani 1 1 d . . .
C51 C 0.2534(3) 0.6720(2) 0.2388(3) 0.0142(5) Uani 1 1 d . . .
O51 O 0.10670(19) 0.68043(16) 0.11339(19) 0.0180(4) Uani 1 1 d . . .
C52 C 0.3950(3) 0.7609(2) 0.2675(3) 0.0189(5) Uani 1 1 d . . .
H52A H 0.4784 0.7219 0.2397 0.028 Uiso 1 1 calc R . .
H52B H 0.4537 0.7862 0.3862 0.028 Uiso 1 1 calc R . .
H52C H 0.3452 0.8324 0.1952 0.028 Uiso 1 1 calc R . .
C61 C 0.1208(3) 0.4093(2) 0.1806(3) 0.0145(5) Uani 1 1 d . . .
O61 O -0.0387(2) 0.36474(17) 0.10291(19) 0.0186(4) Uani 1 1 d . . .
H61 H -0.0487 0.3107 0.0297 0.028 Uiso 1 1 d R . .
O62 O 0.2327(2) 0.38608(17) 0.1438(2) 0.0224(4) Uani 1 1 d . . .
C111 C 0.3325(3) 0.6837(2) 0.8280(3) 0.0202(5) Uani 1 1 d . . .
H11A H 0.2247 0.6761 0.8362 0.024 Uiso 1 1 calc R . .
H11B H 0.4266 0.6440 0.9284 0.024 Uiso 1 1 calc R . .
C112 C 0.3752(3) 0.8181(2) 0.8272(3) 0.0229(5) Uani 1 1 d . . .
H12A H 0.4821 0.8260 0.8195 0.034 Uiso 1 1 calc R . .
H12B H 0.3905 0.8565 0.9317 0.034 Uiso 1 1 calc R . .
H12C H 0.2804 0.8583 0.7300 0.034 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0214(12) 0.0168(12) 0.0133(11) -0.0003(10) 0.0048(10) -0.0021(10)
C2 0.0163(12) 0.0170(13) 0.0222(13) 0.0035(10) 0.0027(10) -0.0025(9)
C3 0.0158(11) 0.0198(13) 0.0252(13) 0.0052(10) 0.0101(11) 0.0018(10)
C4 0.0191(11) 0.0145(12) 0.0168(11) 0.0012(9) 0.0091(10) -0.0002(9)
C4a 0.0138(11) 0.0128(12) 0.0136(11) 0.0021(9) 0.0045(10) -0.0010(8)
N5 0.0120(9) 0.0137(10) 0.0117(9) 0.0010(8) 0.0038(8) -0.0010(7)
C6 0.0117(10) 0.0148(11) 0.0113(10) -0.0002(9) 0.0049(9) -0.0006(8)
C6a 0.0133(11) 0.0176(12) 0.0136(11) 0.0004(9) 0.0071(9) 0.0010(9)
C7 0.0156(11) 0.0201(12) 0.0151(11) -0.0019(9) 0.0061(9) -0.0004(9)
C8 0.0177(12) 0.0162(12) 0.0217(12) 0.0009(10) 0.0085(10) -0.0028(10)
C9 0.0173(12) 0.0222(13) 0.0183(12) 0.0054(10) 0.0097(10) 0.0008(10)
C10 0.0172(12) 0.0242(13) 0.0135(11) -0.0006(10) 0.0069(10) 0.0020(10)
C10a 0.0125(10) 0.0167(11) 0.0162(11) 0.0002(9) 0.0068(9) 0.0006(9)
C11 0.0152(11) 0.0167(12) 0.0135(11) -0.0015(9) 0.0073(9) -0.0009(9)
C11a 0.0184(12) 0.0098(10) 0.0156(11) 0.0006(9) 0.0083(10) -0.0010(9)
C51 0.0168(11) 0.0142(11) 0.0121(11) -0.0020(9) 0.0074(9) 0.0004(9)
O51 0.0161(8) 0.0186(9) 0.0150(8) 0.0025(7) 0.0040(7) 0.0005(7)
C52 0.0207(12) 0.0162(12) 0.0194(12) 0.0029(10) 0.0092(10) -0.0010(10)
C61 0.0176(11) 0.0127(11) 0.0117(10) 0.0022(9) 0.0058(9) 0.0001(9)
O61 0.0176(8) 0.0213(9) 0.0150(8) -0.0065(7) 0.0062(7) -0.0045(7)
O62 0.0221(9) 0.0252(10) 0.0241(9) -0.0062(8) 0.0144(8) -0.0024(7)
C111 0.0243(12) 0.0195(13) 0.0176(12) -0.0036(11) 0.0106(10) -0.0018(11)
C112 0.0265(13) 0.0208(13) 0.0248(13) -0.0065(10) 0.0151(11) -0.0031(10)
#=========================================================================
# 10. Molecular Geometry
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.388(4) . ?
C1 C11a 1.395(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(3) . ?
C3 H3 0.9500 . ?
C4 C4a 1.383(3) . ?
C4 H4 0.9500 . ?
C4a C11a 1.402(3) . ?
C4a N5 1.442(3) . ?
N5 C51 1.354(3) . ?
N5 C6 1.479(3) . ?
C6 C6a 1.538(3) . ?
C6 C61 1.538(3) . ?
C6 H6 1.0000 . ?
C6a C7 1.390(3) . ?
C6a C10a 1.423(3) . ?
C7 C8 1.390(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(3) . ?
C9 H9 0.9500 . ?
C10 C10a 1.401(3) . ?
C10 H10 0.9500 . ?
C10a C11 1.532(3) . ?
C11 C11a 1.533(3) . ?
C11 C111 1.536(3) . ?
C11 H11 1.0000 . ?
C51 O51 1.249(3) . ?
C51 C52 1.506(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O62 1.207(3) . ?
C61 O61 1.328(3) . ?
O61 H61 0.8602 . ?
C111 C112 1.523(4) . ?
C111 H11A 0.9900 . ?
C111 H11B 0.9900 . ?
C112 H12A 0.9800 . ?
C112 H12B 0.9800 . ?
C112 H12C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11a 120.9(2) . . ?
C2 C1 H1 119.5 . . ?
C11a C1 H1 119.5 . . ?
C1 C2 C3 120.7(2) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C4a C4 C3 119.6(2) . . ?
C4a C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C4a C11a 122.1(2) . . ?
C4 C4a N5 120.27(19) . . ?
C11a C4a N5 117.61(19) . . ?
C51 N5 C4a 121.36(18) . . ?
C51 N5 C6 117.57(18) . . ?
C4a N5 C6 121.06(17) . . ?
N5 C6 C6a 114.16(18) . . ?
N5 C6 C61 108.54(17) . . ?
C6a C6 C61 112.80(19) . . ?
N5 C6 H6 107.0 . . ?
C6a C6 H6 107.0 . . ?
C61 C6 H6 107.0 . . ?
C7 C6a C10a 118.7(2) . . ?
C7 C6a C6 119.6(2) . . ?
C10a C6a C6 121.6(2) . . ?
C8 C7 C6a 121.6(2) . . ?
C8 C7 H7 119.2 . . ?
C6a C7 H7 119.2 . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 119.2(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C9 C10 C10a 122.0(2) . . ?
C9 C10 H10 119.0 . . ?
C10a C10 H10 119.0 . . ?
C10 C10a C6a 118.4(2) . . ?
C10 C10a C11 120.5(2) . . ?
C6a C10a C11 120.8(2) . . ?
C10a C11 C11a 103.51(18) . . ?
C10a C11 C111 114.78(19) . . ?
C11a C11 C111 115.41(19) . . ?
C10a C11 H11 107.6 . . ?
C11a C11 H11 107.6 . . ?
C111 C11 H11 107.6 . . ?
C1 C11a C4a 117.4(2) . . ?
C1 C11a C11 125.3(2) . . ?
C4a C11a C11 116.87(19) . . ?
O51 C51 N5 120.3(2) . . ?
O51 C51 C52 121.4(2) . . ?
N5 C51 C52 118.30(19) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O62 C61 O61 125.0(2) . . ?
O62 C61 C6 123.3(2) . . ?
O61 C61 C6 111.64(18) . . ?
C61 O61 H61 110.7 . . ?
C112 C111 C11 111.7(2) . . ?
C112 C111 H11A 109.3 . . ?
C11 C111 H11A 109.3 . . ?
C112 C111 H11B 109.3 . . ?
C11 C111 H11B 109.3 . . ?
H11A C111 H11B 108.0 . . ?
C111 C112 H12A 109.5 . . ?
C111 C112 H12B 109.5 . . ?
H12A C112 H12B 109.5 . . ?
C111 C112 H12C 109.5 . . ?
H12A C112 H12C 109.5 . . ?
H12B C112 H12C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11a C1 C2 C3 -1.3(4) . . . . ?
C1 C2 C3 C4 2.1(4) . . . . ?
C2 C3 C4 C4a -0.1(4) . . . . ?
C3 C4 C4a C11a -2.7(4) . . . . ?
C3 C4 C4a N5 176.0(2) . . . . ?
C4 C4a N5 C51 -70.0(3) . . . . ?
C11a C4a N5 C51 108.7(2) . . . . ?
C4 C4a N5 C6 109.3(2) . . . . ?
C11a C4a N5 C6 -72.0(3) . . . . ?
C51 N5 C6 C6a -158.55(19) . . . . ?
C4a N5 C6 C6a 22.1(3) . . . . ?
C51 N5 C6 C61 74.7(2) . . . . ?
C4a N5 C6 C61 -104.7(2) . . . . ?
N5 C6 C6a C7 -141.2(2) . . . . ?
C61 C6 C6a C7 -16.7(3) . . . . ?
N5 C6 C6a C10a 42.9(3) . . . . ?
C61 C6 C6a C10a 167.43(19) . . . . ?
C10a C6a C7 C8 2.2(3) . . . . ?
C6 C6a C7 C8 -173.8(2) . . . . ?
C6a C7 C8 C9 1.0(4) . . . . ?
C7 C8 C9 C10 -3.0(3) . . . . ?
C8 C9 C10 C10a 1.8(3) . . . . ?
C9 C10 C10a C6a 1.4(3) . . . . ?
C9 C10 C10a C11 -172.7(2) . . . . ?
C7 C6a C10a C10 -3.4(3) . . . . ?
C6 C6a C10a C10 172.6(2) . . . . ?
C7 C6a C10a C11 170.7(2) . . . . ?
C6 C6a C10a C11 -13.4(3) . . . . ?
C10 C10a C11 C11a 108.4(2) . . . . ?
C6a C10a C11 C11a -65.6(3) . . . . ?
C10 C10a C11 C111 -18.3(3) . . . . ?
C6a C10a C11 C111 167.7(2) . . . . ?
C2 C1 C11a C4a -1.4(3) . . . . ?
C2 C1 C11a C11 171.5(2) . . . . ?
C4 C4a C11a C1 3.4(3) . . . . ?
N5 C4a C11a C1 -175.3(2) . . . . ?
C4 C4a C11a C11 -170.1(2) . . . . ?
N5 C4a C11a C11 11.2(3) . . . . ?
C10a C11 C11a C1 -103.1(3) . . . . ?
C111 C11 C11a C1 23.1(4) . . . . ?
C10a C11 C11a C4a 69.8(2) . . . . ?
C111 C11 C11a C4a -163.9(2) . . . . ?
C4a N5 C51 O51 178.7(2) . . . . ?
C6 N5 C51 O51 -0.7(3) . . . . ?
C4a N5 C51 C52 -1.5(3) . . . . ?
C6 N5 C51 C52 179.1(2) . . . . ?
N5 C6 C61 O62 24.4(3) . . . . ?
C6a C6 C61 O62 -103.1(3) . . . . ?
N5 C6 C61 O61 -155.01(18) . . . . ?
C6a C6 C61 O61 77.5(2) . . . . ?
C10a C11 C111 C112 -168.0(2) . . . . ?
C11a C11 C111 C112 71.7(3) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
# Hydrogen bonding scheme
# ======== ======= ======
#
# D H A D-H H...A D...A D-H...A symm publ
# - - - --- ----- ----- ------- ---- ----
O61 H61 O51 0.86 1.83 2.672(2) 167 2_545 no
C2 H2 O51 0.95 2.49 3.309(3) 144 1_656 no
C112 H12A O62 0.98 2.46 3.418(4) 165 2_656 no
#======================================================================
_iucr_refine_instructions_details
;
TITL CM45F8
CELL 0.71073 8.8053 10.9821 9.0080 90.000 118.510 90.000
ZERR 2.00 0.0003 0.0004 0.0006 0.000 0.003 0.000
LATT -1
SYMM - X, 1/2 + Y, - Z
SFAC C H N O
UNIT 38 38 2 6
MERG 4
OMIT -2.00 55.00
FMAP 2
PLAN 20
SIZE 0.10 0.14 0.26
ACTA
BOND $H
CONF
HTAB
OMIT 1 1 0
OMIT -1 1 1
LIST 4
L.S. 8
TEMP -153.00
WGHT 0.035100 0.165700
FVAR 1.39751
C1 1 0.642443 0.594154 0.793875 11.00000 0.02140 0.01683 =
0.01327 -0.00034 0.00478 -0.00213
AFIX 43
H1 2 0.659873 0.615425 0.903129 11.00000 -1.20000
AFIX 0
C2 1 0.782781 0.559463 0.773119 11.00000 0.01629 0.01699 =
0.02217 0.00353 0.00273 -0.00253
AFIX 43
H2 2 0.895282 0.558863 0.867841 11.00000 -1.20000
AFIX 0
C3 1 0.760432 0.525515 0.614880 11.00000 0.01584 0.01980 =
0.02524 0.00519 0.01015 0.00176
AFIX 43
H3 2 0.856262 0.499287 0.601936 11.00000 -1.20000
AFIX 0
C4 1 0.595473 0.530554 0.475729 11.00000 0.01912 0.01446 =
0.01678 0.00125 0.00906 -0.00022
AFIX 43
H4 2 0.577979 0.507917 0.366895 11.00000 -1.20000
AFIX 0
C4a 1 0.457563 0.568724 0.497261 11.00000 0.01382 0.01282 =
0.01356 0.00214 0.00450 -0.00103
N5 3 0.288314 0.581975 0.353266 11.00000 0.01198 0.01373 =
0.01166 0.00100 0.00383 -0.00105
C6 1 0.146917 0.496600 0.324411 11.00000 0.01169 0.01480 =
0.01126 -0.00015 0.00490 -0.00064
AFIX 13
H6 2 0.038938 0.546079 0.283111 11.00000 -1.20000
AFIX 0
C6a 1 0.171355 0.429513 0.484153 11.00000 0.01329 0.01757 =
0.01355 0.00044 0.00709 0.00104
C7 1 0.124326 0.307677 0.473724 11.00000 0.01560 0.02008 =
0.01506 -0.00192 0.00609 -0.00038
AFIX 43
H7 2 0.088369 0.265234 0.370398 11.00000 -1.20000
AFIX 0
C8 1 0.128614 0.246451 0.610695 11.00000 0.01770 0.01619 =
0.02174 0.00087 0.00851 -0.00276
AFIX 43
H8 2 0.097654 0.162826 0.600826 11.00000 -1.20000
AFIX 0
C9 1 0.178015 0.307296 0.761647 11.00000 0.01733 0.02220 =
0.01834 0.00538 0.00971 0.00082
AFIX 43
H9 2 0.175933 0.267006 0.853983 11.00000 -1.20000
AFIX 0
C10 1 0.230502 0.427676 0.776204 11.00000 0.01718 0.02418 =
0.01352 -0.00059 0.00685 0.00203
AFIX 43
H10 2 0.267411 0.468531 0.880811 11.00000 -1.20000
AFIX 0
C10a 1 0.230749 0.490913 0.641243 11.00000 0.01246 0.01667 =
0.01623 0.00016 0.00684 0.00056
C11 1 0.309683 0.618540 0.667747 11.00000 0.01523 0.01672 =
0.01353 -0.00154 0.00732 -0.00093
AFIX 13
H11 2 0.230748 0.669420 0.568637 11.00000 -1.20000
AFIX 0
C11a 1 0.476255 0.598216 0.656614 11.00000 0.01843 0.00976 =
0.01565 0.00055 0.00829 -0.00105
C51 1 0.253368 0.672019 0.238787 11.00000 0.01680 0.01421 =
0.01210 -0.00198 0.00743 0.00042
O51 4 0.106700 0.680430 0.113386 11.00000 0.01608 0.01859 =
0.01499 0.00249 0.00402 0.00048
C52 1 0.395047 0.760869 0.267480 11.00000 0.02070 0.01620 =
0.01940 0.00286 0.00916 -0.00096
AFIX 137
H52A 2 0.478434 0.721879 0.239710 11.00000 -1.50000
H52B 2 0.453745 0.786182 0.386198 11.00000 -1.50000
H52C 2 0.345169 0.832372 0.195207 11.00000 -1.50000
AFIX 0
C61 1 0.120819 0.409307 0.180594 11.00000 0.01761 0.01275 =
0.01168 0.00224 0.00579 0.00012
O61 4 -0.038667 0.364738 0.102914 11.00000 0.01765 0.02128 =
0.01495 -0.00650 0.00617 -0.00452
AFIX 3
H61 2 -0.048669 0.310674 0.029683 11.00000 -1.50000
AFIX 0
O62 4 0.232707 0.386081 0.143759 11.00000 0.02212 0.02519 =
0.02409 -0.00624 0.01436 -0.00241
C111 1 0.332488 0.683745 0.827992 11.00000 0.02428 0.01948 =
0.01756 -0.00357 0.01064 -0.00184
AFIX 23
H11A 2 0.224713 0.676059 0.836195 11.00000 -1.20000
H11B 2 0.426599 0.644010 0.928445 11.00000 -1.20000
AFIX 0
C112 1 0.375182 0.818096 0.827218 11.00000 0.02653 0.02084 =
0.02483 -0.00653 0.01506 -0.00313
AFIX 137
H12A 2 0.482058 0.825982 0.819501 11.00000 -1.50000
H12B 2 0.390518 0.856476 0.931702 11.00000 -1.50000
H12C 2 0.280435 0.858256 0.729953 11.00000 -1.50000
HKLF 4
REM CM45F8
REM R1 = 0.0360 for 1638 Fo > 4sig(Fo) and 0.0455 for all 1851 data
REM 210 parameters refined using 1 restraints
END
WGHT 0.0351 0.1657
REM Highest difference peak 0.209, deepest hole -0.240, 1-sigma level 0.047
Q1 1 0.1374 0.4513 0.2451 11.00000 0.05 0.21
Q2 1 0.5006 0.7306 0.7023 11.00000 0.05 0.18
Q3 1 0.2063 0.4551 0.5588 11.00000 0.05 0.18
Q4 1 0.2180 0.5354 0.3391 11.00000 0.05 0.17
Q5 1 0.6831 0.6851 0.9667 11.00000 0.05 0.17
Q6 1 0.0732 0.0693 0.6018 11.00000 0.05 0.17
Q7 1 0.6020 0.8659 0.3678 11.00000 0.05 0.17
Q8 1 0.5105 0.9084 0.2589 11.00000 0.05 0.16
Q9 1 0.5204 0.7451 0.5750 11.00000 0.05 0.16
Q10 1 0.4683 0.5985 0.5722 11.00000 0.05 0.16
Q11 1 0.6412 0.7835 0.4017 11.00000 0.05 0.15
Q12 1 0.1569 0.5382 0.0448 11.00000 0.05 0.15
Q13 1 0.4688 0.7959 0.5012 11.00000 0.05 0.15
Q14 1 0.7544 0.4002 0.4802 11.00000 0.05 0.15
Q15 1 0.5796 0.8187 0.5697 11.00000 0.05 0.15
Q16 1 0.3044 0.2205 0.6197 11.00000 0.05 0.15
Q17 1 0.1886 0.2243 1.0318 11.00000 0.05 0.15
Q18 1 0.2287 0.7530 0.4991 11.00000 0.05 0.14
Q19 1 0.8512 0.4325 0.9053 11.00000 0.05 0.14
Q20 1 0.5138 0.7749 0.3766 11.00000 0.05 0.14
;
# start Validation Reply Form
_vrf_PUBL005_GLOBAL
;
PROBLEM: _publ_contact_author_email, _publ_contact_author_fax and
RESPONSE: Example CIF
;
# end Validation Reply Form
#======================================================================
# END of CIF
#======================================================================