Synthetic and Structural Studies on the Transition-Metal Fullerene Complexes (η2-C60)M[(η5-Ph2PC5H4)2Ru] and (η2-C60)M[(η5-Ph2PC5H4)2Co]+(PF6)-(M = Pd, Pt) and the Related Compound {[η5-Ph2P(O)C5H4]2Co}+(PF6)-
Song, Li-Cheng; Yu, Guang-Ao; Su, Fu-Hai; Hu, Qing-Mei; Organometallics 23 (2004) 4192–; doi:10.1021/om049667a

data_4076301
_publ_section_title
;
 Synthetic and Structural Studies on the Transition-Metal Fullerene
 Complexes (\h2-C60)M[(\h5-Ph2PC5H4)2Ru] and
 (\h2-C60)M[(\h5-Ph2PC5H4)2Co]+(PF6)-(M = Pd, Pt) and the Related Compound
 {[\h5-Ph2P(O)C5H4]2Co}+(PF6)-
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4192
_journal_paper_doi               10.1021/om049667a
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C106.5 H38.75 Cl2.25 Co F6 P3 Pd'
_chemical_formula_weight         1770.13
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 90.541(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.747(4)
_cell_length_b                   24.155(9)
_cell_length_c                   19.768(6)
_cell_measurement_reflns_used    910
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.73
_cell_measurement_theta_min      2.99
_cell_volume                     7041(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.1110
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29373
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.873205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         11873
_refine_ls_number_restraints     1428
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+3.9171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                6457
_reflns_number_total             11873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049667asi20040512_083957.cif
_cod_data_source_block           030402b
_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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C106.50 H38.75 Cl2.25 Co F6 P3 Pd'
_cod_database_code               4076301