Effect of Heterocycle Content on Metal Binding Isostere Coordination
Dick, Benjamin L.; Patel, Ashay; Cohen, Seth M.; Chemical Science  (2020) –; doi:10.1039/D0SC02717K

data_1558336
_publ_section_title
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 Effect of Heterocycle Content on Metal Binding Isostere Coordination
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02717K
_journal_year                    2020
_chemical_formula_moiety         'C39 H33 B N10 O2 Zn, 1.5(C H4 O)'
_chemical_formula_sum            'C40.5 H39 B N10 O3.5 Zn'
_chemical_formula_weight         797.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2020-04-28 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.7280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1038(7)
_cell_length_b                   18.2437(6)
_cell_length_c                   20.8443(7)
_cell_measurement_reflns_used    6917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.80
_cell_measurement_theta_min      2.18
_cell_volume                     7861.5(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48259
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.697
_diffrn_reflns_theta_min         1.489
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.4903
_exptl_absorpt_correction_T_min  0.4228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0545 before and 0.0483 after correction. The Ratio of minimum to maximum transmission is 0.8623. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             3320
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/methanol/pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         14806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+6.3429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10328
_reflns_number_total             14806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02717k2.cif
_cod_data_source_block           Tp_MePh_Zn_1d
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C40.50 H39 B N10 O3.50 Zn'
_cod_database_code               1558336
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 N17(H17A), N7(H7), C10(H10), C65(H65), C42(H42), C59(H59), C16(H16), C49(H49),
  C52(H52), C74(H74), C66(H66), C62(H62), C13(H13), C23(H23), C67(H67),
 C69(H69), C17(H17), C68(H68), C73(H73), C3(H3), C9(H9), C48(H48), C71(H71),
 C45(H45), C72(H72), C30(H30), C55(H55), C35(H35), C58(H58), C46(H46), C6(H6),
 C8(H8), C18(H18), C7(H7A), C26(H26), C47(H47), C57(H57), C56(H56), C34(H34),
 C20(H20), C27(H27), C32(H32), C29(H29), C28(H28), C33(H33), C19(H19)
2.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C50(H50A,H50B,H50C), C21(H21A,H21B,H21C), C40(H40A,H40B,
 H40C), C11(H11A,H11B,H11C), C1(H1A,H1B,H1C), C80(H80A,H80B,H80C), C79(H79A,
 H79B,H79C), C81(H81A,H81B,H81C)
2.d Idealised tetrahedral OH refined as rotating group:
 O6(H6A), O5(H5), O7(H7B)
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_shelx_res_checksum              70783
_shelx_hkl_checksum              53970
_olex2_submission_special_instructions 'No special instructions were received'