Valence tautomerism in a cobalt–dioxolene complex containing an imidazolic ancillary ligand
Moledo Vicente Guedes, Anderson; Sodré de Abreu, Leandro; Maldonado, Igor Antunes Vogel; Fernandes, William Silva; Cardozo, Thiago Messias; A. Allão Cassaro, Rafael; Scarpellini, Marciela; Poneti, Giordano; RSC Advances 13 (2023) 20050–20057; doi:10.1039/D3RA03235C

data_7246985
_publ_section_title
;
 Valence tautomerism in a cobalt--dioxolene complex containing an
 imidazolic ancillary ligand
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              20050
_journal_page_last               20057
_journal_paper_doi               10.1039/D3RA03235C
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C31 H42 Co N6 O2, F6 P, 3[H2O], 3[CH4O]'
_chemical_formula_sum            'C34 H60 Co F6 N6 O8 P'
_chemical_formula_weight         884.788
_chemical_properties_physical    'desolvation of lattice solvents'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2023-05-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-05-14 deposited with the CCDC.	2023-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.93(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.945(4)
_cell_length_b                   15.221(5)
_cell_length_c                   22.683(10)
_cell_measurement_reflns_used    1969
_cell_measurement_temperature    132.05
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.40
_cell_volume                     4388(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      132.05
_diffrn_measured_fraction_theta_full 0.7895
_diffrn_measured_fraction_theta_max 0.7895
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.1825
_diffrn_reflns_Laue_measured_fraction_full 0.7895
_diffrn_reflns_Laue_measured_fraction_max 0.7895
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9405
_diffrn_reflns_point_group_measured_fraction_full 0.7895
_diffrn_reflns_point_group_measured_fraction_max 0.7895
_diffrn_reflns_theta_full        25.0233
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.505
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1867.004
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         1.1834
_refine_diff_density_min         -1.1993
_refine_diff_density_rms         0.1471
_refine_ls_d_res_high            0.8401
_refine_ls_d_res_low             6.8599
_refine_ls_goodness_of_fit_ref   1.0241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6125
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.0227
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2878
_refine_ls_wR_factor_ref         0.3425
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3280
_reflns_number_total             6125
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ra03235c2.cif
_cod_data_source_block           mo_cobimapy35dicat01_6_0m
_cod_original_formula_sum        'C34 Co1 F6 H60 N6 O8 P1 '
_cod_database_code               7246985
_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
 P-F2
 1.571 with sigma of 0.02
 P-F3
 1.571 with sigma of 0.02
 P-F5
 1.571 with sigma of 0.02
 P-F6
 1.571 with sigma of 0.02
 P-F2A
 1.571 with sigma of 0.02
 P-F3A
 1.571 with sigma of 0.02
 P-F5A
 1.571 with sigma of 0.02
 P-F6A
 1.571 with sigma of 0.02
 F2-F3 \\sim F3-F5 \\sim F5-F6 \\sim F6-F2 \\sim F2A-F3A \\sim F3A-F5A \\sim
F5A-F6A \\sim F6A-F2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F3) = Uanis(F2) = Uanis(F5) = Uanis(F6) = Uanis(F3A) = Uanis(F2A) =
Uanis(F5A) = Uanis(F6A)
4. Others
 Fixed Sof: F3(0.59623) F5(0.59623) F6(0.59623) F2(0.59623) F5A(0.40377)
 F2A(0.40377) F3A(0.40377) F6A(0.40377)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27a,H27b), C21(H21a,H21b), C20(H20a,H20b), C19(H19a,H19b)
5.b Me refined with riding coordinates:
 C00S(H00a,H00b,H00c), C13(H13a,H13b,H13c), C01B(H01a,H01b,H01c), C8(H8a,H8b,
 H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C14(H14a,H14b,H14c), C11(H11a,H11b,
 H11c)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C4(H4), C6(H6), C17(H17), C23(H23), C30(H30), C26(H26), C29(H29),
 C24(H24), C25(H25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'