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_1558335
_publ_section_title
;
 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 H36 B N9 O2 Zn, 1.5(C6 H6)'
_chemical_formula_sum            'C48 H45 B N9 O2 Zn'
_chemical_formula_weight         856.11
_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             2020-02-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-28 deposited with the CCDC.	2020-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.044(11)
_cell_angle_beta                 90.661(10)
_cell_angle_gamma                117.154(13)
_cell_formula_units_Z            4
_cell_length_a                   11.951(7)
_cell_length_b                   12.222(7)
_cell_length_c                   33.40(2)
_cell_measurement_reflns_used    6498
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.33
_cell_measurement_theta_min      2.27
_cell_volume                     4307(4)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0983
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            61119
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.226
_diffrn_reflns_theta_max         24.226
_diffrn_reflns_theta_min         1.229
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.4894
_exptl_absorpt_correction_T_min  0.4414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0619 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.9012. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       plate
_exptl_crystal_F_000             1788
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/pentane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         13796
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+5.6819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9145
_reflns_number_total             13796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02717k2.cif
_cod_data_source_block           Tp_MePh_Zn_2a
_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               1558335
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All B(H,H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N14A) = Uanis(N14)
Uanis(N15A) = Uanis(N15)
Uanis(C60A) = Uanis(C60)
Uanis(C61A) = Uanis(C61)
Uanis(C62) = Uanis(C62A)
Uanis(C63A) = Uanis(C63)
Uanis(C64A) = Uanis(C64)
3. Rigid body (RIGU) restrains
 C96A, C91A, H91A, C92A, H96A, C95A, H92A, C93A, H95A, C94A, H93A, H94A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C96, H96, C95, H91, C92, C94, H95, C93, H92, H94, H93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, C61, N14, N15, C62, C63, C64, C69, C68, C67, C66, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 N14A, N15A, C63A, C62A, C61A, C60A, C64A, C69A, C68A, C67A, C66A, C65A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C91A)=Sof(H91A)=Sof(C96A)=Sof(H96A)=Sof(C95A)=Sof(H95A)=Sof(C94A)=
 Sof(H94A)=Sof(C92A)=Sof(H92A)=Sof(C93A)=Sof(H93A)=1-FVAR(1)
 Sof(C96)=Sof(H96)=Sof(C91)=Sof(H91)=Sof(C94)=Sof(H94)=Sof(C93)=Sof(H93)=
 Sof(C95)=Sof(H95)=Sof(C92)=Sof(H92)=FVAR(1)
 Sof(H2B)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(N14A)=
 Sof(N15A)=Sof(C63A)=Sof(C62A)=Sof(H62A)=Sof(C64A)=Sof(C69A)=Sof(H69A)=
 Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=Sof(C65A)=
 Sof(H65A)=1-FVAR(2)
 Sof(H2A)=Sof(N14)=Sof(N15)=Sof(C61)=Sof(C63)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C62)=Sof(H62)=Sof(C64)=Sof(C69)=Sof(H69)=Sof(C68)=Sof(H68)=
 Sof(C67)=Sof(H67)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2A), B2(H2B)
5.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N17(H17), C42(H42), C23(H23), C3(H3), C74(H74), C10(H10), C38(H38),
 C49(H49), C45(H45), C55(H55), C47(H47), C77(H77), C6(H6), C52(H52), C13(H13),
 C46(H46), C35(H35), C48(H48), C20(H20), C57(H57), C9(H9), C75(H75), C29(H29),
 C36(H36), C26(H26), C37(H37), C19(H19), C76(H76), C30(H30), C56(H56), C8(H8A),
 C7(H7), C81(H81), C59(H59), C80(H80), C16(H16), C28(H28), C87(H87), C83(H83),
 C27(H27), C79(H79), C58(H58), C18(H18), C17(H17A), C86(H86), C82(H82),
 C88(H88), C84(H84), C85(H85), C90(H90), C89(H89), C96(H96), C91(H91), C94(H94),
  C93(H93), C95(H95), C92(H92), C91A(H91A), C96A(H96A), C95A(H95A), C94A(H94A),
 C92A(H92A), C93A(H93A), C62(H62), C69(H69), C68(H68), C67(H67), C65(H65),
 C66(H66), C62A(H62A), C69A(H69A), C68A(H68A), C67A(H67A), C66A(H66A),
 C65A(H65A)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C40(H40A,H40B,H40C), C1(H1A,H1B,
 H1C), C31(H31A,H31B,H31C), C50(H50A,H50B,H50C), C70(H70A,H70B,H70C), C60(H60A,
 H60B,H60C), C60A(H60D,H60E,H60F)
;
_shelx_res_checksum              52517
_shelx_hkl_checksum              51973
_olex2_submission_special_instructions 'No special instructions were received'