Syntheses, crystal structures and catalytic activities of two solvent-induced homotrinuclear Co(ii) complexes with a naphthalenediol-based bis(Salamo)-type tetraoxime ligand
Li, Xiao-Yan; Chen, Le; Gao, Lei; Zhang, Yang; Akogun, Sunday Folaranmi; Dong, Wen-Kui; RSC Adv. 7 (2017) 35905–; doi:10.1039/C7RA06796H

data_7228699
_publ_section_title
;
 Syntheses, crystal structures and catalytic activities of two
 solvent-induced homotrinuclear Co(ii) complexes with a
 naphthalenediol-based bis(Salamo)-type tetraoxime ligand
;
_journal_issue                   57
_journal_name_full               'RSC Adv.'
_journal_page_first              35905
_journal_paper_doi               10.1039/C7RA06796H
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C36 H34 Br4 Co3 N4 O14, 2(C H Cl3)'
_chemical_formula_sum            'C38 H36 Br4 Cl6 Co3 N4 O14'
_chemical_formula_weight         1481.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-10-07 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                113.715(9)
_cell_angle_beta                 90.013(7)
_cell_angle_gamma                108.037(7)
_cell_formula_units_Z            2
_cell_length_a                   14.5421(10)
_cell_length_b                   14.8347(13)
_cell_length_c                   17.3221(18)
_cell_measurement_reflns_used    3253
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0460
_cell_measurement_theta_min      3.6580
_cell_volume                     3219.6(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.1319
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21805
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.529
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88634
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1454
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         12621
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0804P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6203
_reflns_number_total             12621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06796h2.cif
_cod_data_source_block           d656-sr
_cod_original_cell_volume        3219.6(5)
_cod_database_code               7228699
_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, All O(H) groups
2. Restrained distances
 O13-H13
 0.85 with sigma of 0.01
 O14-H14
 0.85 with sigma of 0.01
 C36-H13
 1.915447 with sigma of 0.02
 Co2-H13
 2.788011 with sigma of 0.02
 C35-H14
 1.894763 with sigma of 0.02
 Co2-H14
 2.75527 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C38(H38), C37(H37)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C22(H22A,H22B), C23(H23A,H23B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19),
 C21(H21), C24(H24), C28(H28), C30(H30)
3.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'