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_7228698
_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         'C34 H30 Br4 Co3 N4 O14'
_chemical_formula_sum            'C34 H30 Br4 Co3 N4 O14'
_chemical_formula_weight         1215.05
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-23 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.6144(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.182(2)
_cell_length_b                   18.751(2)
_cell_length_c                   18.722(2)
_cell_measurement_reflns_used    2119
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.6120
_cell_measurement_theta_min      3.7770
_cell_volume                     6170.1(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35080
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.434
_exptl_absorpt_correction_T_max  0.5187
_exptl_absorpt_correction_T_min  0.4464
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.136
_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     552
_refine_ls_number_reflns         11495
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                7713
_reflns_number_total             11495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra06796h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        6169.9(12)
_cod_database_code               7228698
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br3') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: Br2(0.8) Br3(0.7) Br2'(0.2) Br3'(0.3)
4.a Riding coordinates:
 O14(H14A,H14B), O13(H13A,H13B)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C22(H22A,H22B), C23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C19(H19), C18(H18), C17(H17), C16(H16),
 C21(H21), C24(H24), C30(H30), C28(H28)
4.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'