Reactivity of a Phosphido-Niobocene Derivative toward CS2 and Alkyl Halides to Give Phosphinodithioformato- and Phosphino-Niobocene Complexes: X-ray Crystal Structures of [Nb(η5-C5H4SiMe3)2(κ1-S-SC(S)(PPh2))(CO)] and [Nb(η5-C5H4SiMe3)2(P(I)Ph2)(CO)]I3
Antiñolo, Antonio; García-Yuste, Santiago; Otero, Antonio; Pérez-Flores, Juan C.; Reguillo-Carmona, Rebeca; Rodríguez, Ana M.; Villaseñor, Elena; Organometallics 25 (2006) 1310–1316; doi:10.1021/om051013u

data_4074930
_publ_section_title
;
 Reactivity of a Phosphido-Niobocene Derivative toward CS2 and Alkyl
 Halides to Give Phosphinodithioformato- and Phosphino-Niobocene
 Complexes: X-ray Crystal Structures of
 [Nb(\h5-C5H4SiMe3)2(\k1-S-SC(S)(PPh2))(CO)] and
 [Nb(\h5-C5H4SiMe3)2(P(I)Ph2)(CO)]I3
;
_journal_coden_ASTM              ORGND7
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1310
_journal_page_last               1316
_journal_paper_doi               10.1021/om051013u
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C30 H36 Nb O P S2 Si2'
_chemical_formula_weight         656.77
_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                 108.76(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.063(8)
_cell_length_b                   10.834(8)
_cell_length_c                   18.488(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     3236(3)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q 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  0.0914
_diffrn_reflns_av_sigmaI/netI    0.3987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7656
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.21
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.3249
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                1715
_reflns_number_total             7413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051013usi20051124_044713.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'psi scan' changed to
'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4074930