An Unusally Diverse Array of Products Formed upon Carbonylation of a Dialkylniobium Complex
Neil C. Tomson; Andrew Yan; John Arnold; Robert G. Bergman; Journal of the American Chemical Society 130 (2008) 11262–11263; doi:10.1021/ja803729k

data_4108246
_publ_contact_author_address
;Department of Chemistry
University of California at Berkeley
Berkeley, CA 94720-1460 (USA)
;
_publ_contact_author_email       arnold@berkeley.edu
_publ_contact_author_name        'Prof. John Arnold'
_publ_contact_author_phone       (+1)510-643-5181
_publ_section_title
;
 An Unusally Diverse Array of Products Formed upon Carbonylation of a
 Dialkylniobium Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11262
_journal_page_last               11263
_journal_paper_doi               10.1021/ja803729k
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C44 H65 N4 Nb'
_chemical_formula_sum            'C44 H65 N4 Nb'
_chemical_formula_weight         742.91
_chemical_name_common            (BDI)(XylNCMe2)Nb(NCMe3)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                99.359(3)
_cell_angle_beta                 93.498(3)
_cell_angle_gamma                94.676(3)
_cell_formula_units_Z            2
_cell_length_a                   12.253(3)
_cell_length_b                   13.004(3)
_cell_length_c                   13.033(3)
_cell_measurement_reflns_used    1899
_cell_measurement_temperature    119(2)
_cell_measurement_theta_max      43.717
_cell_measurement_theta_min      6.613
_cell_volume                     2036.4(8)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.054d'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_molecular_graphics    'Bruker-AXS XP v.6'
_computing_publication_material  'Bruker-AXS XP v.6'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      119(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'SMART 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10381
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.896711
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                4866
_reflns_number_total             6674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803729k-file007.cif
_cod_data_source_block           n5c55txs1
_cod_database_code               4108246