Remarkable organophosphorus cage compounds from the reaction of cobaltocene and the triphosphole P3C2But2CH(SiMe3) 2: crystal and molecular structures of [Co(η5-C5H5)(η4-C 4H4CHCHP6C4But 4)] and P6C4But4CH(SiMe3)
Hitchcock, Peter B.; Nixon, John F.; Büyükkidan, Nurgün Sakarya; Chemical Communications  (2001) 2720–; doi:10.1039/b108125j

data_7125523
_publ_section_title
;
 Remarkable organophosphorus cage compounds from the reaction of
 cobaltocene and the triphosphole P3C2But2CH(SiMe3) 2: crystal and
 molecular structures of [Co(\h5-C5H5)(\h4-C 4H4CHCHP6C4But 4)] and
 P6C4But4CH(SiMe3)
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2720
_journal_paper_doi               10.1039/b108125j
_journal_year                    2001
_chemical_formula_moiety         'C31 H47 Co P6'
_chemical_formula_sum            'C31 H47 Co P6'
_chemical_formula_weight         664.44
_chemical_name_common            '[Co(Cp)(CpP6cage)]'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.16(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.634(3)
_cell_length_b                   32.706(7)
_cell_length_c                   10.510(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3278.1(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega-2theta scan'
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0948
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6120
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   'psi-scan data'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.567
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_obs          0.0563
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+6.1285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1553
_refine_ls_wR_factor_obs         0.1187
_reflns_number_observed          3897
_reflns_number_total             5769
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108125j.txt
_cod_data_source_block           feb897
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+6.1285P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+6.1285P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7125523