Reactions of Neutral and Cationic Diamide-Supported Imido Complexes with CO <sub>2</sub> and Other Heterocumulenes: Issues of Site Selectivity
Ward, Benjamin D.; Orde, Gavin; Clot, Eric; Cowley, Andrew R.; Gade, Lutz H.; Mountford, Philip; Organometallics 24 (2005) 2368–2385; doi:10.1021/om0500265

data_1100895
_publ_section_title
;
 Reactions of Neutral and Cationic Diamide-Supported Imido Complexes with
 CO <sub>2</sub> and Other Heterocumulenes:&#x2009; Issues of Site
 Selectivity
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2368
_journal_page_last               2385
_journal_paper_doi               10.1021/om0500265
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         ' C24 H47 Cl N5 Nb O Si2 '
_chemical_formula_sum            'C24 H47 Cl N5 Nb O Si2'
_chemical_formula_weight         606.21
_chemical_melting_point          ?
_chemical_name_systematic
;
 [Nb(NtBu){MeC(2-C5H4N)(CH2NSiMe3)(CH2NC(OSiMe3)NtBu)}Cl]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 100.7414(6)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.8425(3)
_cell_length_b                   21.5100(4)
_cell_length_c                   36.4135(7)
_cell_measurement_reflns_used    70472
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     12960.8
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            70472
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' pale yellow '
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             5089.006
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.50
_refine_ls_goodness_of_fit_ref   1.0441
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         12358
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.041017
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979)
 1.02    0.284    0.702
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0501
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              47
_reflns_limit_l_min              0
_reflns_number_gt                12358
_reflns_number_total             25778
_reflns_threshold_expression     >3.00\s(I)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C24 H47 Cl N5 Nb O Si2 '
_cod_database_code               1100895