Sterically Encumbered Systems for Two Low-Coordinate Phosphorus Centers
Shashin Shah; Tom E. Concolino; Arnold L. Rheingold; John D. Protasiewicz; Inorganic Chemistry 39 (2000) 3860–3867; doi:10.1021/ic0001558

data_4321259
_publ_contact_author
; 
     Dr. J. D. Protasiewicz 
     Department of Chemistry 
     402NA Millis Science Center
     Case Western Reserve University
     10900 Euclid Avenue 
     Cleveland, OH 44106-7078 
;
_publ_contact_author_email       jdp5@po.cwru.edu
_publ_contact_author_fax         '+216 368 3006'
_publ_contact_author_phone       '+216 368 5060'
_publ_section_title
;
 Sterically Encumbered Systems for Two Low-Coordinate Phosphorus Centers
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3860
_journal_page_last               3867
_journal_paper_doi               10.1021/ic0001558
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C96 H102 Cl6 D2 P4'
_chemical_formula_weight         1596.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.3505(7)
_cell_angle_beta                 75.9850(10)
_cell_angle_gamma                74.4804(11)
_cell_formula_units_Z            1
_cell_length_a                   11.8495(2)
_cell_length_b                   13.0427(2)
_cell_length_c                   16.1474(2)
_cell_measurement_temperature    233(2)
_cell_volume                     2329.18(6)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11568
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.9166
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.507
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+6.0133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2691
_reflns_number_gt                4776
_reflns_number_total             6362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0001558_2.cif
_cod_data_source_block           pro04
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
;
_cod_original_cell_volume        2329.19(5)
_cod_database_code               4321259