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_1558341
_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         '2(C38 H33 B N12 Zn), 5(C3 H3)'
_chemical_formula_sum            'C91 H81 B2 N24 Zn2'
_chemical_formula_weight         1663.15
_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             2020-01-28
_audit_creation_method
;
Olex2 1.2
(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                111.296(6)
_cell_angle_beta                 101.338(4)
_cell_angle_gamma                94.752(4)
_cell_formula_units_Z            2
_cell_length_a                   14.290(3)
_cell_length_b                   16.009(4)
_cell_length_c                   20.236(5)
_cell_measurement_reflns_used    9711
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.19
_cell_volume                     4168.4(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0635
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.342
_diffrn_reflns_theta_min         1.385
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.4912
_exptl_absorpt_correction_T_min  0.4410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1108 before and 0.0733 after correction. The Ratio of minimum to maximum transmission is 0.8978. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             1730
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/methanol/pentane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         16899
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0289P)^2^+2.7904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14493
_reflns_number_total             16899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02717k2.cif
_cod_data_source_block           Tp_MePh_Zn_2c
_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_cell_volume        4168.3(16)
_cod_database_code               1558341
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.832
_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
2. Restrained distances
 C98-C97 \\sim C98A-C97A
 with sigma of 0.02
 C98-C93 \\sim C98A-C93A
 with sigma of 0.02
 C95-C96 \\sim C95A-C96A
 with sigma of 0.02
 C95-C94 \\sim C95A-C94A
 with sigma of 0.02
 C96-C97 \\sim C96A-C97A
 with sigma of 0.02
 C94-C93 \\sim C94A-C93A
 with sigma of 0.02
 C98-C96 \\sim C98A-C96A
 with sigma of 0.04
 C98-C94 \\sim C98A-C94A
 with sigma of 0.04
 C95-C97 \\sim C95A-C97A
 with sigma of 0.04
 C95-C93 \\sim C95A-C93A
 with sigma of 0.04
 C96-C94 \\sim C96A-C94A
 with sigma of 0.04
 C97-C93 \\sim C97A-C93A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C98) = Uanis(C95) = Uanis(C96) = Uanis(C94) = Uanis(C97) = Uanis(C93)
Uanis(C93A) = Uanis(C98A) = Uanis(C97A) = Uanis(C96A) = Uanis(C94A) =
Uanis(C95A)
4. Rigid body (RIGU) restrains
 C95, C98, C97, C93, C96, C94
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C87, C92, C91, C90, C88, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C93A)=Sof(H93A)=Sof(C98A)=Sof(H98A)=Sof(C97A)=Sof(H97A)=Sof(C96A)=
 Sof(H96A)=Sof(C94A)=Sof(H94A)=Sof(C95A)=Sof(H95A)=1-FVAR(1)
 Sof(C98)=Sof(H98)=Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96)=Sof(C94)=Sof(H94)=
 Sof(C97)=Sof(H97)=Sof(C93)=Sof(H93)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
6.b Aromatic/amide H refined with riding coordinates:
 N20(H20A), N8(H8), C33(H33), C40(H40), C83(H83), C61(H61), C71(H71), C51(H51),
  C36(H36), C45(H45), C68(H68), C30(H30), C64(H64), C23(H23), C54(H54),
 C44(H44), C80(H80), C42(H42), C13(H13), C65(H65), C81(H81), C74(H74), C26(H26),
  C43(H43), C58(H58), C39(H39), C55(H55), C82(H82), C16(H16), C78(H78),
 C38(H38), C57(H57), C67(H67), C20(H20), C66(H66), C37(H37), C75(H75), C17(H17),
  C29(H29), C56(H56), C77(H77), C101(H101), C18(H18), C27(H27), C99(H99),
 C19(H19), C100(H100), C76(H76), C28(H28), C98(H98), C92(H92), C91(H91),
 C90(H90), C95(H95), C96(H96), C94(H94), C97(H97), C93(H93), C89(H89), C87(H87),
  C88(H88), C93A(H93A), C98A(H98A), C97A(H97A), C96A(H96A), C94A(H94A),
 C95A(H95A)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C59(H59A,H59B,H59C), C31(H31A,H31B,H31C), C69(H69A,H69B,
 H69C), C49(H49A,H49B,H49C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              69794
_shelx_hkl_checksum              68744
_olex2_submission_special_instructions 'No special instructions were received'