Coordinatively- and Electronically-Unsaturated Square Planar Cobalt(III) Complexes of a Pyridine Dianionic Pincer Ligand
Hana, Faidh; Lough, Alan; Lavoie, Gino G.; Dalton Transactions  (2017) –; doi:10.1039/C7DT03674D

data_7044631
_publ_section_title
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 Coordinatively- and Electronically-Unsaturated Square Planar Cobalt(III)
 Complexes of a Pyridine Dianionic Pincer Ligand
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03674D
_journal_year                    2017
_chemical_formula_moiety         'C32 H38 Co N4, B F4'
_chemical_formula_sum            'C32 H38 B Co F4 N4'
_chemical_formula_weight         624.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-10-26 deposited with the CCDC.
2017-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.597(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.9885(16)
_cell_length_b                   11.9621(8)
_cell_length_c                   19.1699(13)
_cell_measurement_reflns_used    8087
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      24.32
_cell_measurement_theta_min      2.21
_cell_volume                     6181.8(7)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      147.14
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41569
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_min         1.511
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0650 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.9212.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5689
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0472P)^2^+16.9082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3853
_reflns_number_total             5689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03674d2.cif
_cod_data_source_block           d16121
_cod_database_code               7044631
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F4
 1.34 with sigma of 0.06
 B2-F5 = B2-F6 = B2-F7 = B2-F8
 1.34 with sigma of 0.06
 F5-F6 = F6-F7 = F7-F8 = F8-F5 = F7-F5 = F8-F6
 2.21 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F4 \\sim F4-F1 \\sim F3-F1 \\sim F4-F2
 with sigma of 0.01
3. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) B1(0.5) F5(0.5) F6(0.5) F7(0.5)
 F8(0.5) B2(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              65096
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'