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_1558354
_publ_section_title
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 Effect of Heterocycle Content on Metal Binding Isostere Coordination
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02717K
_journal_year                    2020
_chemical_formula_moiety         'C39 H35 B N8 O3 Zn, C6 H6'
_chemical_formula_sum            'C45 H41 B N8 O3 Zn'
_chemical_formula_weight         818.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-29 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                100.704(3)
_cell_angle_beta                 96.654(3)
_cell_angle_gamma                114.105(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7292(11)
_cell_length_b                   11.9654(12)
_cell_length_c                   16.3974(16)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.38
_cell_volume                     2016.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_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_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53797
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         2.028
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.4908
_exptl_absorpt_correction_T_min  0.4564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0477 before and 0.0393 after correction. The Ratio of minimum to maximum transmission is 0.9299. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/pentane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8246
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+1.2432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7397
_reflns_number_total             8246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02717k2.cif
_cod_data_source_block           Tp_MePh_Zn_5a
_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_database_code               1558354
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C40, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C40A, C41A, C42A, C43A, C44A, C45A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C40A)=
 Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=1-FVAR(1)
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C40)=Sof(H40)=
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 B1(H1)
4.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C6(H6), C23(H23), C13(H13), C20(H20), C30(H30), C10(H10), C7(H7),
 C35(H35), C3(H3), C9(H9), C29(H29), C8(H8), C17(H17), C37(H37), C36(H36),
 C16(H16), C28(H28), C19(H19), C18(H18), C26(H26), C27(H27), C43(H43), C44(H44),
  C45(H45), C40(H40), C41(H41), C42(H42), C43A(H43A), C44A(H44A), C45A(H45A),
 C40A(H40A), C41A(H41A), C42A(H42A)
4.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C40,C41,C42), C43A(C44A,C45A,C40A,C41A,C42A)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              12633
_shelx_hkl_checksum              39650
_olex2_submission_special_instructions 'No special instructions were received'