Synthesis, Characterization, and Reactivity of Isocyanidephosphidoniobocene Derivatives: X-ray Diffraction Structures of New Isocyanideniobocene Complexes, [Nb(η5-C5H4SiMe3)2(CNR)(PMePh2)]I, R = Xylyl, Cy
Antiñolo, Antonio; Evrard, David; García-Yuste, Santiago; Otero, Antonio; Pérez-Flores, Juan C.; Reguillo-Carmona, Rebeca; Rodríguez, Ana M.; Villaseñor, Elena; Organometallics 25 (2006) 3670–; doi:10.1021/om060283p

data_4075444
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of
 Isocyanidephosphidoniobocene Derivatives:&#x00A0; X-ray Diffraction
 Structures of New Isocyanideniobocene Complexes,
 [Nb(\h5-C5H4SiMe3)2(CNR)(PMePh2)]I, R = Xylyl, Cy
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3670
_journal_paper_doi               10.1021/om060283p
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C38 H48 I N Nb P Si2'
_chemical_formula_weight         825.73
_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                   10.992(5)
_cell_length_b                   14.390(2)
_cell_length_c                   24.683(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     3904.2(19)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, Cascarano, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.1134
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9411
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.03
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.709
_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   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+1.1227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1956
_reflns_number_gt                4723
_reflns_number_total             9411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060283psi20060330_115755.cif
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4075444