An Organometallic Radical Route to Bis(phosphido)- and Hydrido−Phosphido-Bridged Metal−Metal-Bonded Complexes of Cyclopentadienylchromium via Desulfurization of Thiophosphinito Ligands
Goh, Lai Yoong; Weng, Zhiqiang; Leong, Weng Kee; Vittal, Jagadese J.; Haiduc, Ionel; Organometallics 21 (2002) 5287–; doi:10.1021/om0203680

data_4084048
_publ_section_title
;
 An Organometallic Radical Route to Bis(phosphido)- and
 Hydrido&#x2212;Phosphido-Bridged Metal&#x2212;Metal-Bonded Complexes of
 Cyclopentadienylchromium via Desulfurization of Thiophosphinito Ligands
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5287
_journal_paper_doi               10.1021/om0203680
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C19 H21 Cr3 O2 P S'
_chemical_formula_weight         500.39
_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                 106.0710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.6524(5)
_cell_length_b                   27.9082(14)
_cell_length_c                   15.5775(8)
_cell_measurement_reflns_used    7320
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.19
_cell_volume                     4032.3(4)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            64531
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.781
_exptl_absorpt_correction_T_max  0.746076
_exptl_absorpt_correction_T_min  0.582990
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         12281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                9631
_reflns_number_total             12281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0203680.cif
_cod_data_source_block           compd_5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4084048