Filling the gap with a bulky diaryl boron group: fluorinated and non-fluorinated copper pyrazolates fitted with a dimesityl boron moiety on the backbone
Vanga, Mukundam; Diroll, Benjamin T.; Muñoz-Castro, Alvaro; Dias, Rasika; Dalton Transactions  (2023) –; doi:10.1039/D3DT03167E

data_7714135
_publ_section_title
;
 Filling the gap with a bulky diaryl boron group: fluorinated and
 non-fluorinated copper pyrazolates fitted with a dimesityl boron moiety
 on the backbone
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03167E
_journal_year                    2023
_chemical_formula_moiety         'C69 H84 B3 Cu3 N6, C7 H15'
_chemical_formula_sum            'C76 H99 B3 Cu3 N6'
_chemical_formula_weight         1319.66
_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             2023-02-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-08-09 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                109.624(2)
_cell_angle_beta                 93.285(2)
_cell_angle_gamma                105.508(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9999(5)
_cell_length_b                   16.1430(5)
_cell_length_c                   17.2755(6)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.54
_cell_volume                     3496.8(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Photon II 7 CPAD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Photon II 7'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'Photon II 7 CPAD'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56142
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0479 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.8795.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             1398
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         21160
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0562P)^2^+2.7433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16790
_reflns_number_total             21160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03167e2.cif
_cod_data_source_block           hrd84_0m_a
_cod_database_code               7714135
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C70-C71 = C72I-C71 = C72-C71 = C72I-C73I = C73-C72 = C73I-C74I = C73-C74 =
 C75I-C74I = C74-C75 = C75I-C76I = C76-C75
 1.53 with sigma of 0.01
 C70-C71 \\sim C72I-C71 \\sim C72-C71 \\sim C72I-C73I \\sim C73-C72 \\sim
C73I-C74I \\sim C73-C74 ~
 C75I-C74I \\sim C74-C75 \\sim C76-C75 \\sim C75I-C76I
 with sigma of 0.008
3. Others
 Fixed Sof: H71A(0.5) H71B(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) C74(0.5) H74A(0.5) H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5)
 C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5) C72I(0.5) H72C(0.5) H72D(0.5) C73I(0.5)
 H73C(0.5) H73D(0.5) C74I(0.5) H74C(0.5) H74D(0.5) C75I(0.5) H75C(0.5)
 H75D(0.5) C76I(0.5) H76D(0.5) H76E(0.5) H76F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C72I(H72C,H72D), C73I(H73C,H73D), C74I(H74C,H74D), C75I(H75C,H75D)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C17(H17), C19(H19), C31(H31), C33(H33), C40(H40), C42(H42),
 C54(H54), C56(H56), C63(H63), C65(H65)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C76(H76A,H76B,H76C),
 C76I(H76D,H76E,H76F)
;
_shelx_res_checksum              97124
_olex2_submission_special_instructions 'No special instructions were received'