Competitive Insertion of Isocyanide and Carbon Dioxide into Niobium− and Silicon−Amido Bonds
Alcalde, M. Isabel; Gómez-Sal, M. Pilar; Royo, Pascual; Organometallics 20 (2001) 4623–; doi:10.1021/om0103963

data_4077368
_publ_section_title
;
 Competitive Insertion of Isocyanide and Carbon Dioxide into
 Niobium&#x2212; and Silicon&#x2212;Amido Bonds
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4623
_journal_paper_doi               10.1021/om0103963
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C11 H19 Cl N Nb O Si'
_chemical_formula_weight         337.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.240(10)
_cell_angle_beta                 80.970(10)
_cell_angle_gamma                81.650(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4370(10)
_cell_length_b                   8.8180(10)
_cell_length_c                   11.8190(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     744.25(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2840
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        'not significant'
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_type   'not made'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             344
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .22
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.3461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                2471
_reflns_number_total             2620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0103963.cif
_cod_data_source_block           mabel31
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077368