1,2,3,4-Tetraphenyl-1,2,3,4-tetraphospholane, a Highly Versatile Cyclocarbaphosphine Ligand: Reactions with Activated Triosmium Clusters and Characterization of the Products
Siau-Gek Ang; Zhong; How-Ghee Ang; Inorganic Chemistry 41 (2002) 3791–3800; doi:10.1021/ic025589c

data_4318224
_publ_section_title
;
 1,2,3,4-Tetraphenyl-1,2,3,4-tetraphospholane, a Highly Versatile
 Cyclocarbaphosphine Ligand: Reactions with Activated Triosmium Clusters
 and Characterization of the Products
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3791
_journal_page_last               3800
_journal_paper_doi               10.1021/ic025589c
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C41.5 H26.5 Cl1.5 O16 Os6 P4'
_chemical_formula_weight         2099.38
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.32
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.0038(3)
_cell_length_b                   13.5080(2)
_cell_length_c                   21.68700(10)
_cell_measurement_reflns_used    22161
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      1.81
_cell_volume                     5932.35(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22161
_diffrn_reflns_theta_full        29.39
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    26.064
_exptl_absorpt_correction_T_max  0.187316
_exptl_absorpt_correction_T_min  0.101465
_exptl_absorpt_correction_type   'Sadabs (sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.701
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.364
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.264
_refine_ls_extinction_coef       0.000044(8)
_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   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+163.4057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                5592
_reflns_number_total             7200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025589c_8.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_cell_volume        5932.18(12)
_cod_original_formula_sum        'C41.50 H26.50 Cl1.50 O16 Os6 P4'
_cod_database_code               4318224