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_1558355
_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         'C38 H32 B N7 O3 Zn, 0.5(C6 H6), 0.5(C5 H12)'
_chemical_formula_sum            'C43.5 H41 B N7 O3 Zn'
_chemical_formula_weight         786.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-29
_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                90
_cell_angle_beta                 106.120(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5694(12)
_cell_length_b                   14.5978(11)
_cell_length_c                   17.7711(14)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.48
_cell_volume                     3880.2(5)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_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  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.4908
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0494 before and 0.0437 after correction. The Ratio of minimum to maximum transmission is 0.9089. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/methanol/pentane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         7655
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0386P)^2^+4.0557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5831
_reflns_number_total             7655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02717k2.cif
_cod_data_source_block           Tp_MePh_Zn_5
_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        'C43.50 H41 B N7 O3 Zn'
_cod_database_code               1558355
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained planarity
 C46, C44, C49, C45, C48, C47
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C44) = Uanis(C40)
Uanis(C42) = Uanis(C46)
4. Rigid body (RIGU) restrains
 C48, C49, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C48(0.5) H2(0.5) C47(0.5) H6(0.5) C46(0.5) H0AA(0.5) C45(0.5)
 H4(0.5) C44(0.5) H1(0.5) C49(0.5) H3(0.5) C41(0.5) H3AA(0.5) H3AB(0.5)
 C42(0.5) H4AA(0.5) H4AB(0.5) C43(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) C39(0.5)
 H1AA(0.5) H1AB(0.5) H1AC(0.5) C40(0.5) H2AA(0.5) H2AB(0.5)
6.a Ternary CH refined with riding coordinates:
 B1(H01N)
6.b Secondary CH2 refined with riding coordinates:
 C41(H3AA,H3AB), C42(H4AA,H4AB), C40(H2AA,H2AB)
6.c Aromatic/amide H refined with riding coordinates:
 C29(H00O), C20(H00M), C13(H00I), C23(H00J), C19(H00U), C30(H00N), C27(H00T),
 C28(H00V), C34(H00X), C10(H00Z), C26(H00K), C9(H01A), C36(H01C), C17(H01D),
 C18(H01B), C16(H011), C3(H013), C37(H015), C7(H016), C8(H017), C35(H018),
 C6(H019), C48(H2), C47(H6), C46(H0AA), C45(H4), C44(H1), C49(H3)
6.d Fitted hexagon refined as free rotating group:
 C48(C47,C46,C45,C44,C49)
6.e Idealised Me refined as rotating group:
 C21(H01E,H01F,H01G), C11(H01H,H01I,H01J), C1(H01K,H01L,H01M), C43(H5AA,H5AB,
 H5AC), C39(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              65054
_shelx_hkl_checksum              77636
_olex2_submission_special_instructions 'No special instructions were received'