Tris(<i>tert</i>-butyl isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(I) perchlorate dichloromethane disolvate and tris(<i>tert</i>-butyl isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(II) bis(perchlorate) dichloromethane disolvate: modification of a trigonal‒bipyramidal structure with change of metal oxidation state
Becker, Clifford A. L.; Black, Robert S.; Forbes, Roy P.; Acta Crystallographica Section C 66 (2010) m40–m43; doi:10.1107/S0108270109054626

data_2017536
_publ_section_title
;
 Tris(<i>tert</i>-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(I) perchlorate
 dichloromethane disolvate and tris(<i>tert</i>-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(II)
 bis(perchlorate) dichloromethane disolvate: modification of a
 trigonal--bipyramidal structure with change of metal oxidation state
;
_journal_coeditor_code           TR3058
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m40
_journal_page_last               m43
_journal_paper_doi               10.1107/S0108270109054626
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Co (C5 H9 N)3 (C21 H21 O3 P)2] (Cl O4)2, 2C H2 Cl2'
_chemical_formula_moiety
'C57 H69 Co N3 O6 P2 2+, 2(Cl O4 -), 2(C H2 Cl2)'
_chemical_formula_sum            'C59 H73 Cl6 Co N3 O14 P2'
_chemical_formula_weight         1381.77
_chemical_name_systematic
;Tris(<i>tert</i>-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(II)
bis(perchlorate)
 dichloromethane disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3461(3)
_cell_length_b                   19.7566(5)
_cell_length_c                   28.4452(7)
_cell_measurement_reflns_used    7487
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.18
_cell_volume                     6929.9(3)
_computing_cell_refinement       'SAINT-NT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-NT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            93953
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2876
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.408
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         16738
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+6.8607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                11549
_reflns_number_total             16738
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr3058.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017536
_cod_database_fobs_code          2017536