Synthesis and molecular structures of a pair of tris(imidazolyl)phosphine cobalt–perchlorate complexes, {[PimPri2]Co(OClO3)}[ClO4] and {[PimPri2]Co(OH2)(HOMe)(OClO3)}[ClO4]
Kimblin, Clare; Bridgewater, Brian M.; Churchill, David G.; Parkin, Gerard; Journal of the Chemical Society, Dalton Transactions  (2000) 2191–; doi:10.1039/b002894k

data_7009708
_publ_section_title
;
 Synthesis and molecular structures of a pair of
 tris(imidazolyl)phosphine cobalt--perchlorate complexes,
 {[PimPri2]Co(OClO3)}[ClO4] and {[PimPri2]Co(OH2)(HOMe)(OClO3)}[ClO4]
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2191
_journal_paper_doi               10.1039/b002894k
_journal_year                    2000
_chemical_formula_sum            'C29 H47 Cl8 Co N6 O8 P'
_chemical_formula_weight         981.23
_space_group_IT_number           14
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3832(11)
_cell_length_b                   16.8991(12)
_cell_length_c                   17.8228(11)
_cell_measurement_temperature    238(2)
_cell_volume                     4560.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      238(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31912
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_T_min  0.7681
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         10147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+1.5503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                6201
_reflns_number_total             10147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002894k.txt
_cod_data_source_block           cobs10
_cod_database_code               7009708