A mixed-valence complex of cobalt based on 3-methoxysalicylaldoxime
Yao, Tiantian; Lu, Jing; Li, Dacheng; Dou, Jianmin; Acta Crystallographica Section C 70 (2014) 364–367; doi:10.1107/S2053229614005245

data_2019441
_publ_section_title
;
 A mixed-valence complex of cobalt based on 3-methoxysalicylaldoxime
;
_journal_coeditor_code           SF3224
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              364
_journal_page_last               367
_journal_paper_doi               10.1107/S2053229614005245
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Co4 (C8 H7 N O3)2 (C8 H8 N O3)2 (N3)4 (C2 H6 O)2] , 2C2 H6 O'
_chemical_formula_moiety         'C36 H42 Co4 N16 O14, 2(C2 H6 O)'
_chemical_formula_sum            'C40 H54 Co4 N16 O16'
_chemical_formula_weight         1250.71
_chemical_name_systematic
'Di-\m~2~-azido-diazidodiethanolbis{\m~2~-2-[(hydroxyimino)methyl]-6-methoxyphenolato}bis{\m~3~-2-[(oxidoimino)methyl]-6-methoxyphenolato}dicobalt(II)dicobalt(III) ethanol disolvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                91.524(11)
_cell_angle_beta                 107.539(10)
_cell_angle_gamma                93.855(10)
_cell_formula_units_Z            1
_cell_length_a                   9.605(7)
_cell_length_b                   10.749(7)
_cell_length_c                   13.010(9)
_cell_measurement_reflns_used    931
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.743
_cell_measurement_theta_min      2.234
_cell_volume                     1276.3(15)
_computing_cell_refinement       'SMART (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.1595
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6405
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.9108
_exptl_absorpt_correction_T_min  0.7631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.621
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                2144
_reflns_number_total             4419
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3224sup1.cf
_cod_data_source_block           I
_cod_database_code               2019441
_cod_database_fobs_code          2019441