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_4318219
_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            'C51 H31 Cl2 O22 Os6 P4'
_chemical_formula_weight         2331.74
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4535(2)
_cell_length_b                   24.78720(10)
_cell_length_c                   39.05110(10)
_cell_measurement_reflns_used    39338
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.29
_cell_volume                     13022.5(2)
_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 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            39338
_diffrn_reflns_theta_full        29.41
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    11.913
_exptl_absorpt_correction_T_max  0.467286
_exptl_absorpt_correction_T_min  0.198362
_exptl_absorpt_correction_type   'sadabs (Sheldric, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.000007(4)
_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   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+71.2524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                5813
_reflns_number_total             8347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025589c_3.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
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_cod_database_code               4318219