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_4084044
_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            'C11 H15 Cr O2 P S'
_chemical_formula_weight         294.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   6.98970(10)
_cell_length_b                   13.2350(2)
_cell_length_c                   14.0795(3)
_cell_measurement_reflns_used    3573
_cell_measurement_temperature    193(2)
_cell_volume                     1302.48(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_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  0.1213
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9246
_diffrn_reflns_theta_full        28.83
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.862145
_exptl_absorpt_correction_T_min  0.318246
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                1195
_reflns_number_total             1838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0203680.cif
_cod_data_source_block           compd_2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      P212121
_cod_database_code               4084044