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_4075443
_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            'C36 H50 I N Nb P Si2'
_chemical_formula_weight         803.73
_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                 97.400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.143(5)
_cell_length_b                   14.3220(10)
_cell_length_c                   24.444(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      2
_cell_volume                     3868.5(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0351
_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       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9299
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.20
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9299
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.3686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1851
_reflns_number_gt                6064
_reflns_number_total             9299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060283psi20060330_115755.cif
_cod_data_source_block           11
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4075443