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_2017537
_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(C H2 Cl2)'
_chemical_formula_moiety         'C57 H69 Co N3 O6 P2 +, Cl O4 -, 2(C H2 Cl2)'
_chemical_formula_sum            'C59 H73 Cl5 Co N3 O10 P2'
_chemical_formula_weight         1282.32
_chemical_name_systematic
;Tris(<i>tert</i>-butyl
 isocyanide)bis[tris(4-methoxyphenyl)phosphine]cobalt(I)
perchlorate
 dichloromethane disolvate
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.7568(3)
_cell_length_b                   21.7568(3)
_cell_length_c                   23.3983(6)
_cell_measurement_reflns_used    7171
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.56
_cell_volume                     9591.9(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0583
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46534
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.8087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4020
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+16.3243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.152
_reflns_number_gt                4167
_reflns_number_total             6456
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr3058.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               2017537
_cod_database_fobs_code          2017537