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_7009709
_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 H55 Cl2 Co N6 O11 P'
_chemical_formula_weight         824.59
_chemical_name_systematic
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 ? 
;
_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'
_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                 90.5370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6185(8)
_cell_length_b                   18.2452(11)
_cell_length_c                   17.6528(10)
_cell_measurement_temperature    233(2)
_cell_volume                     4064.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28024
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.9377
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9302
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          4.172
_refine_ls_shift/su_mean         0.172
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+2.6687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                7543
_reflns_number_total             9302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002894k.txt
_cod_data_source_block           pims10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009709