Not so inert <i>mer</i>-tris-chelate cobalt(III) complex of a hydroxy-pyridine functionalized NHC ligand for cyclic carbonate synthesis.
Chowdhury, Rhitwika; Bhat, Irshad Ahmad; Sachan, Sharad Kumar; Anantharaman, Ganapathi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17157–17161; doi:10.1039/d4dt02767a

data_7717211
_publ_section_title
;
 Not so inert <i>mer</i>-tris-chelate cobalt(III) complex of a
 hydroxy-pyridine functionalized NHC ligand for cyclic carbonate
 synthesis.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17157
_journal_page_last               17161
_journal_paper_doi               10.1039/d4dt02767a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C27 H25 Co N9 O3, 4.865(H2 O), 1.5[H2O]'
_chemical_formula_sum            'C27 H34 Co N9 O8.5'
_chemical_formula_weight         679.56
_chemical_name_systematic        Co1
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.895(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5150(6)
_cell_length_b                   17.8418(12)
_cell_length_c                   19.7536(14)
_cell_measurement_reflns_used    5120
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.37
_cell_volume                     2979.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_unetI/netI     0.1123
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21547
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         2.507
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6315
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0862 before and 0.0601 after correction. The Ratio of minimum to maximum transmission is 0.8469. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'metallic dark gray'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.8429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3234
_reflns_number_total             5267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02767a2.cif
_cod_data_source_block           3sepb_0m
_cod_depositor_comments          'Adding full bibliography for 7717211.cif.'
_cod_original_formula_sum        'C27 H34 Co N9 O8.50'
_cod_database_code               7717211
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.882
_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, All O(H,H) groups
2. Others
 Fixed Sof: O5(0.5)
3.a Free rotating group:
 O9(H9D,H9E), O8(H8A,H8B), O4(H4A,H4B), O7(H7A,H7B), O6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C21(H21), C20(H20), C26(H26), C15(H15), C24(H24),
 C25(H25), C12(H12), C8(H8), C3(H3), C6(H6), C2(H2), C11(H11), C7(H7)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              22008
_shelx_hkl_checksum              65058
_olex2_submission_special_instructions 'No special instructions were received'