# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_KurkMa1901
_audit_block_doi 10.5517/ccdc.csd.cc22f5yn
_database_code_depnum_ccdc_archive 'CCDC 1919301'
loop_
_audit_author_name
_audit_author_address
'Victor Rybakov'
;Chemistry Department Moscow State University
Russia
;
_audit_update_record
;
2019-05-28 deposited with the CCDC. 2019-11-18 downloaded from the CCDC.
;
_chemical_name_systematic
(E)-5-((4-bromophenyl)((difluoroboranyl)amino)methylene)-2,3-dimethyl-3,5-dihydro-4H-imidazol-4-one
_chemical_name_common ?
_chemical_melting_point_gt 501
_chemical_melting_point_lt 503
_chemical_formula_moiety 'C12 H11 B Br F2 N3 O'
_chemical_formula_sum 'C12 H11 B Br F2 N3 O'
_chemical_formula_weight 341.96
_exptl_crystal_description prism
_exptl_crystal_colour 'light yellow'
_exptl_crystal_density_diffrn 1.731
_exptl_crystal_preparation CH~~3CN
_cell_length_a 4.8377(6)
_cell_length_b 9.7590(13)
_cell_length_c 14.1241(19)
_cell_angle_alpha 82.194(11)
_cell_angle_beta 85.642(10)
_cell_angle_gamma 84.183(10)
_cell_volume 655.92(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 295(2)
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x+, y+, z+'
'-x+, -y+, -z+'
_diffrn_ambient_temperature 295(2)
_refine_ls_R_factor_all 0.2383
_refine_ls_R_factor_gt 0.0615
_refine_ls_wR_factor_ref 0.1490
_refine_ls_wR_factor_gt 0.1056
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
BR44 Br 1.5193(2) 0.29400(9) 0.92317(7) 0.0743(4) Uani 1 1 d . . . . .
O1 O 0.2543(9) 0.8310(5) 0.5611(3) 0.0553(14) Uani 1 1 d . . . . .
B2 B 0.418(2) 0.7167(10) 0.5192(7) 0.054(2) Uani 1 1 d . . . . .
F21 F 0.2426(8) 0.6267(4) 0.4965(3) 0.0694(13) Uani 1 1 d . . . . .
F22 F 0.5615(9) 0.7713(5) 0.4358(3) 0.0772(13) Uani 1 1 d . . . . .
N3 N 0.6337(12) 0.6393(6) 0.5887(4) 0.0530(16) Uani 1 1 d . . . . .
H3 H 0.7476 0.5759 0.5667 0.064 Uiso 1 1 calc R U . . .
C4 C 0.6615(14) 0.6602(7) 0.6785(6) 0.0464(18) Uani 1 1 d . . . . .
C4A C 0.4804(14) 0.7663(7) 0.7107(5) 0.0403(17) Uani 1 1 d . . . . .
N5 N 0.4378(12) 0.8158(6) 0.8013(4) 0.0515(16) Uani 1 1 d . . . . .
C6 C 0.2326(15) 0.9128(6) 0.7932(5) 0.0428(18) Uani 1 1 d . . . . .
C61 C 0.0942(16) 0.9856(8) 0.8719(5) 0.072(2) Uani 1 1 d . . . . .
H61A H -0.0507 1.0524 0.8472 0.108 Uiso 1 1 calc R U . . .
H61B H 0.0153 0.9193 0.9203 0.108 Uiso 1 1 calc R U . . .
H61C H 0.2284 1.0322 0.8992 0.108 Uiso 1 1 calc R U . . .
N7 N 0.1341(11) 0.9354(5) 0.7011(4) 0.0415(14) Uani 1 1 d . . . . .
C71 C -0.0848(14) 1.0373(7) 0.6631(5) 0.058(2) Uani 1 1 d . . . . .
H71A H -0.1632 1.0907 0.7125 0.087 Uiso 1 1 calc R U . . .
H71B H -0.0076 1.0980 0.6107 0.087 Uiso 1 1 calc R U . . .
H71C H -0.2276 0.9902 0.6410 0.087 Uiso 1 1 calc R U . . .
C7A C 0.2898(14) 0.8421(7) 0.6508(5) 0.0386(17) Uani 1 1 d . . . . .
C41 C 0.8735(13) 0.5724(7) 0.7353(5) 0.0390(17) Uani 1 1 d . . . . .
C42 C 0.9277(14) 0.6046(7) 0.8241(5) 0.0486(19) Uani 1 1 d . . . . .
H42 H 0.8287 0.6808 0.8477 0.058 Uiso 1 1 calc R U . . .
C43 C 1.1269(15) 0.5251(7) 0.8786(5) 0.052(2) Uani 1 1 d . . . . .
H43 H 1.1683 0.5497 0.9369 0.062 Uiso 1 1 calc R U . . .
C44 C 1.2610(14) 0.4098(8) 0.8447(6) 0.051(2) Uani 1 1 d . . . . .
C45 C 1.2123(15) 0.3735(8) 0.7586(6) 0.057(2) Uani 1 1 d . . . . .
H45 H 1.3080 0.2954 0.7365 0.069 Uiso 1 1 calc R U . . .
C46 C 1.0178(15) 0.4552(8) 0.7050(5) 0.058(2) Uani 1 1 d . . . . .
H46 H 0.9820 0.4306 0.6460 0.070 Uiso 1 1 calc R U . . .
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
BR44 0.0763(7) 0.0594(6) 0.0865(7) 0.0015(4) -0.0334(5) 0.0030(4)
O1 0.064(4) 0.051(3) 0.050(3) -0.017(3) -0.009(3) 0.015(3)
B2 0.048(6) 0.057(6) 0.057(7) -0.012(5) -0.014(5) 0.009(5)
F21 0.065(3) 0.063(3) 0.085(3) -0.031(2) -0.022(2) 0.013(2)
F22 0.077(3) 0.087(3) 0.056(3) 0.007(2) 0.010(2) 0.016(3)
N3 0.061(4) 0.050(4) 0.049(4) -0.020(3) -0.001(3) 0.010(3)
C4 0.038(5) 0.034(4) 0.067(6) -0.005(4) 0.005(4) -0.007(4)
C4A 0.044(5) 0.028(4) 0.048(5) -0.005(4) -0.005(4) 0.002(3)
N5 0.071(5) 0.039(4) 0.046(4) -0.017(3) -0.007(3) 0.005(3)
C6 0.057(5) 0.020(4) 0.052(5) -0.016(3) 0.003(4) -0.001(4)
C61 0.085(6) 0.062(5) 0.070(6) -0.022(5) -0.004(5) 0.012(5)
N7 0.037(4) 0.035(3) 0.051(4) -0.008(3) 0.006(3) 0.004(3)
C71 0.055(5) 0.044(4) 0.074(5) -0.013(4) -0.015(4) 0.019(4)
C7A 0.043(5) 0.031(4) 0.043(5) -0.007(4) 0.008(4) -0.014(3)
C41 0.027(4) 0.039(4) 0.053(5) -0.012(4) 0.005(4) -0.008(3)
C42 0.051(5) 0.036(4) 0.060(5) -0.013(4) 0.000(4) -0.007(4)
C43 0.071(6) 0.038(4) 0.049(5) -0.010(4) -0.009(4) -0.008(4)
C44 0.040(5) 0.057(5) 0.061(5) -0.016(4) -0.012(4) -0.004(4)
C45 0.051(5) 0.047(5) 0.072(6) -0.003(4) 0.000(5) -0.004(4)
C46 0.060(5) 0.062(5) 0.055(5) -0.020(4) -0.010(4) 0.009(4)
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
BR44 C44 1.911(7) . ?
O1 C7A 1.311(7) . ?
O1 B2 1.468(10) . ?
B2 F21 1.365(10) . ?
B2 F22 1.389(10) . ?
B2 N3 1.555(10) . ?
N3 C4 1.331(8) . ?
N3 H3 0.8600 . ?
C4 C4A 1.389(9) . ?
C4 C41 1.479(9) . ?
C4A C7A 1.387(8) . ?
C4A N5 1.421(8) . ?
N5 C6 1.300(7) . ?
C6 N7 1.400(8) . ?
C6 C61 1.482(9) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
N7 C7A 1.362(8) . ?
N7 C71 1.458(7) . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
C41 C46 1.380(9) . ?
C41 C42 1.384(8) . ?
C42 C43 1.385(9) . ?
C42 H42 0.9300 . ?
C43 C44 1.366(9) . ?
C43 H43 0.9300 . ?
C44 C45 1.355(9) . ?
C45 C46 1.374(9) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
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
C7A O1 B2 117.2(6) . . ?
F21 B2 F22 108.8(7) . . ?
F21 B2 O1 109.2(7) . . ?
F22 B2 O1 108.6(7) . . ?
F21 B2 N3 110.3(7) . . ?
F22 B2 N3 108.4(7) . . ?
O1 B2 N3 111.4(7) . . ?
C4 N3 B2 127.2(6) . . ?
C4 N3 H3 116.4 . . ?
B2 N3 H3 116.4 . . ?
N3 C4 C4A 114.9(6) . . ?
N3 C4 C41 119.6(7) . . ?
C4A C4 C41 125.6(7) . . ?
C7A C4A C4 120.5(7) . . ?
C7A C4A N5 107.7(6) . . ?
C4 C4A N5 131.8(6) . . ?
C6 N5 C4A 106.0(5) . . ?
N5 C6 N7 112.4(6) . . ?
N5 C6 C61 125.8(7) . . ?
N7 C6 C61 121.5(6) . . ?
C6 C61 H61A 109.5 . . ?
C6 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C6 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C7A N7 C6 105.7(5) . . ?
C7A N7 C71 125.4(6) . . ?
C6 N7 C71 129.0(6) . . ?
N7 C71 H71A 109.5 . . ?
N7 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
N7 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O1 C7A N7 123.3(6) . . ?
O1 C7A C4A 128.5(7) . . ?
N7 C7A C4A 108.2(6) . . ?
C46 C41 C42 117.3(6) . . ?
C46 C41 C4 122.8(7) . . ?
C42 C41 C4 119.8(7) . . ?
C41 C42 C43 121.2(7) . . ?
C41 C42 H42 119.4 . . ?
C43 C42 H42 119.4 . . ?
C44 C43 C42 118.5(7) . . ?
C44 C43 H43 120.7 . . ?
C42 C43 H43 120.7 . . ?
C45 C44 C43 122.3(7) . . ?
C45 C44 BR44 119.1(6) . . ?
C43 C44 BR44 118.6(6) . . ?
C44 C45 C46 118.2(7) . . ?
C44 C45 H45 120.9 . . ?
C46 C45 H45 120.9 . . ?
C45 C46 C41 122.4(7) . . ?
C45 C46 H46 118.8 . . ?
C41 C46 H46 118.8 . . ?
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
C7A O1 B2 F21 115.3(7) . . . . ?
C7A O1 B2 F22 -126.1(6) . . . . ?
C7A O1 B2 N3 -6.8(10) . . . . ?
F21 B2 N3 C4 -115.9(8) . . . . ?
F22 B2 N3 C4 125.0(8) . . . . ?
O1 B2 N3 C4 5.6(12) . . . . ?
B2 N3 C4 C4A -2.0(11) . . . . ?
B2 N3 C4 C41 177.8(7) . . . . ?
N3 C4 C4A C7A -0.3(9) . . . . ?
C41 C4 C4A C7A 179.9(6) . . . . ?
N3 C4 C4A N5 177.1(7) . . . . ?
C41 C4 C4A N5 -2.7(12) . . . . ?
C7A C4A N5 C6 0.7(7) . . . . ?
C4 C4A N5 C6 -176.9(7) . . . . ?
C4A N5 C6 N7 -1.2(7) . . . . ?
C4A N5 C6 C61 173.5(7) . . . . ?
N5 C6 N7 C7A 1.3(7) . . . . ?
C61 C6 N7 C7A -173.7(6) . . . . ?
N5 C6 N7 C71 -177.7(6) . . . . ?
C61 C6 N7 C71 7.3(10) . . . . ?
B2 O1 C7A N7 -174.0(7) . . . . ?
B2 O1 C7A C4A 5.8(10) . . . . ?
C6 N7 C7A O1 179.1(6) . . . . ?
C71 N7 C7A O1 -1.9(10) . . . . ?
C6 N7 C7A C4A -0.8(7) . . . . ?
C71 N7 C7A C4A 178.3(6) . . . . ?
C4 C4A C7A O1 -1.8(11) . . . . ?
N5 C4A C7A O1 -179.8(6) . . . . ?
C4 C4A C7A N7 178.0(6) . . . . ?
N5 C4A C7A N7 0.1(7) . . . . ?
N3 C4 C41 C46 -10.1(10) . . . . ?
C4A C4 C41 C46 169.7(7) . . . . ?
N3 C4 C41 C42 171.9(6) . . . . ?
C4A C4 C41 C42 -8.3(10) . . . . ?
C46 C41 C42 C43 2.5(10) . . . . ?
C4 C41 C42 C43 -179.4(6) . . . . ?
C41 C42 C43 C44 -3.0(10) . . . . ?
C42 C43 C44 C45 2.2(11) . . . . ?
C42 C43 C44 BR44 -176.3(5) . . . . ?
C43 C44 C45 C46 -1.0(11) . . . . ?
BR44 C44 C45 C46 177.5(5) . . . . ?
C44 C45 C46 C41 0.5(11) . . . . ?
C42 C41 C46 C45 -1.2(10) . . . . ?
C4 C41 C46 C45 -179.3(6) . . . . ?
###########################################################################
_audit_creation_method SHELXL-2015/1
_shelx_SHELXL_version_number 2015/1
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_cell_measurement_reflns_used 29448
_cell_measurement_theta_min 2.115
_cell_measurement_theta_max 28.712
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 340
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.200
_exptl_absorpt_coefficient_mu 3.155
_shelx_estimated_absorpt_T_min 0.571
_shelx_estimated_absorpt_T_max 0.571
_exptl_absorpt_correction_type refdelf
_exptl_absorpt_factor_muR 0.315
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D. (1983) Acta. Cryst. A39, 158-166
;
_exptl_absorpt_correction_T_min 0.6812
_exptl_absorpt_correction_T_max 0.7294
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'LFF Sealed Tube'
_diffrn_detector 'Hybride pixel array detector'
_diffrn_detector_type 'DECTRIS Pilatus--100K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_source_voltage 50
_diffrn_source_current 40
_diffrn_source_power 2.000
_diffrn_source 'SEIFERT Iso--Debyeflex 3003'
_diffrn_measurement_device 'Four cyrcle diffractometer'
_diffrn_measurement_device_type STADI--VARY
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_monochromator 'Plane graphite'
_diffrn_radiation_polarisn_norm 0
_diffrn_radiation_collimation '0.5 mm diameter, monocapillary'
_diffrn_measurement_method 'Rotation method'
_diffrn_measurement_details
;
99 runs, 1524 frames, detector distance = 42 mm
;
_diffrn_reflns_number 3318
_diffrn_reflns_av_unetI/netI 0.2450
_diffrn_reflns_av_R_equivalents 0.0513 # before absorption correction
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.115
_diffrn_reflns_theta_max 28.712
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total 3318
_reflns_number_gt 871
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'X--AREA (STOE & CIE, 2015)'
_computing_cell_refinement 'X--AREA (STOE & CIE, 2015)'
_computing_data_reduction 'X--AREA (STOE & CIE, 2015)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2015/1 (Sheldrick, 2015)'
_computing_molecular_graphics 'Ortep--3 (Farrugia, 1997)'
_computing_publication_material 'WinGX (Farrugia, 1999)'
_refine_special_details ?
_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^)+(0.0555P)^2^] 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 .
_refine_ls_number_reflns 3318
_refine_ls_number_parameters 181
_refine_ls_number_restraints 0
_refine_ls_goodness_of_fit_ref 0.756
_refine_ls_restrained_S_all 0.756
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.351
_refine_diff_density_min -0.436
_refine_diff_density_rms 0.093
_shelx_res_file
;
TITL kurkma1901 in P-1
KurkMa1901.res created by SHELXL-2015/1 at 14:53:37 on 27-Apr-2019
CELL 0.71073 4.8377 9.7590 14.1241 82.194 85.642 84.183
ZERR 2.000 0.0006 0.0013 0.0019 0.011 0.010 0.010
LATT 1
SFAC C H B N O F BR
UNIT 24 22 2 6 2 4 2
TEMP 22
SIZE 0.2 0.2 0.2
L.S. 5
FMAP 2
PLAN 5
BOND $H
EQIV $1 -x+1, -y+1, -z+1
HTAB N3 F21_$1
EQIV $2 -x+1, -y+2, -z+1
HTAB C71 F22_$2
EQIV $3 -x+2, -y+1, -z+1
HTAB C45 F22_$3
ACTA
CONF
WGHT 0.055500
FVAR 0.99456
BR44 7 1.519312 0.294000 0.923170 11.00000 0.07629 0.05937 =
0.08651 0.00155 -0.03343 0.00297
O1 5 0.254322 0.831036 0.561133 11.00000 0.06421 0.05109 =
0.05008 -0.01715 -0.00886 0.01475
B2 3 0.418118 0.716679 0.519156 11.00000 0.04842 0.05746 =
0.05712 -0.01166 -0.01445 0.00897
F21 6 0.242607 0.626738 0.496484 11.00000 0.06519 0.06293 =
0.08512 -0.03129 -0.02223 0.01279
F22 6 0.561536 0.771278 0.435844 11.00000 0.07668 0.08750 =
0.05590 0.00666 0.00966 0.01573
N3 4 0.633721 0.639271 0.588716 11.00000 0.06074 0.04996 =
0.04854 -0.02019 -0.00090 0.00991
AFIX 43
H3 2 0.747629 0.575925 0.566705 11.00000 -1.20000
AFIX 0
C4 1 0.661467 0.660198 0.678518 11.00000 0.03792 0.03351 =
0.06679 -0.00485 0.00487 -0.00694
C4A 1 0.480406 0.766283 0.710689 11.00000 0.04447 0.02773 =
0.04813 -0.00530 -0.00532 0.00219
N5 4 0.437767 0.815772 0.801260 11.00000 0.07144 0.03916 =
0.04559 -0.01691 -0.00735 0.00503
C6 1 0.232649 0.912753 0.793168 11.00000 0.05748 0.02014 =
0.05235 -0.01596 0.00337 -0.00057
C61 1 0.094222 0.985578 0.871915 11.00000 0.08464 0.06155 =
0.06965 -0.02220 -0.00397 0.01163
AFIX 33
H61A 2 -0.050716 1.052444 0.847232 11.00000 -1.50000
H61B 2 0.015346 0.919315 0.920328 11.00000 -1.50000
H61C 2 0.228353 1.032156 0.899203 11.00000 -1.50000
AFIX 0
N7 4 0.134055 0.935376 0.701145 11.00000 0.03670 0.03489 =
0.05100 -0.00845 0.00561 0.00378
C71 1 -0.084767 1.037253 0.663097 11.00000 0.05467 0.04378 =
0.07418 -0.01289 -0.01466 0.01855
AFIX 33
H71A 2 -0.163226 1.090691 0.712510 11.00000 -1.50000
H71B 2 -0.007586 1.097968 0.610717 11.00000 -1.50000
H71C 2 -0.227566 0.990177 0.641011 11.00000 -1.50000
AFIX 0
C7A 1 0.289765 0.842125 0.650815 11.00000 0.04261 0.03132 =
0.04291 -0.00681 0.00840 -0.01444
C41 1 0.873498 0.572435 0.735279 11.00000 0.02736 0.03874 =
0.05260 -0.01229 0.00473 -0.00846
C42 1 0.927718 0.604563 0.824133 11.00000 0.05086 0.03644 =
0.06040 -0.01276 0.00026 -0.00673
AFIX 43
H42 2 0.828741 0.680821 0.847714 11.00000 -1.20000
AFIX 0
C43 1 1.126861 0.525110 0.878564 11.00000 0.07108 0.03797 =
0.04884 -0.00999 -0.00891 -0.00817
AFIX 43
H43 2 1.168338 0.549712 0.936879 11.00000 -1.20000
AFIX 0
C44 1 1.260968 0.409825 0.844692 11.00000 0.03950 0.05731 =
0.06106 -0.01574 -0.01176 -0.00448
C45 1 1.212293 0.373525 0.758637 11.00000 0.05140 0.04680 =
0.07207 -0.00254 -0.00032 -0.00376
AFIX 43
H45 2 1.307982 0.295389 0.736483 11.00000 -1.20000
AFIX 0
C46 1 1.017764 0.455238 0.704965 11.00000 0.05972 0.06170 =
0.05468 -0.02016 -0.00974 0.00936
AFIX 43
H46 2 0.982013 0.430648 0.646032 11.00000 -1.20000
AFIX 0
HKLF 4
REM kurkma1901 in P-1
REM R1 = 0.0615 for 871 Fo > 4sig(Fo) and 0.2383 for all 3318 data
REM 181 parameters refined using 0 restraints
END
WGHT 0.0551 0.0000
REM Highest difference peak 0.351, deepest hole -0.436, 1-sigma level 0.093
Q1 1 -0.1802 0.9742 0.8733 11.00000 0.05 0.35
Q2 1 1.7928 0.3277 0.9590 11.00000 0.05 0.35
Q3 1 0.6855 0.7372 0.9401 11.00000 0.05 0.33
Q4 1 1.5755 0.2690 0.9355 11.00000 0.05 0.31
Q5 1 1.3007 0.2947 0.9652 11.00000 0.05 0.31
;
_shelx_res_checksum 27419