Synthesis and structural characterization of new organo-diimido and organo-imido niobium and titanium complexes
Dorado, Iván; Garcés, Andrés; López-Mardomingo, Carmen; Fajardo, Mariano; Rodríguez, Ana; Antiñolo, Antonio; Otero, Antonio; Journal of the Chemical Society, Dalton Transactions  (2000) 2375–; doi:10.1039/b002743j

data_7009689
_publ_section_title
;
 Synthesis and structural characterization of new organo-diimido and
 organo-imido niobium and titanium complexes
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2375
_journal_paper_doi               10.1039/b002743j
_journal_year                    2000
_chemical_formula_sum            'C17 H38 N2 Nb Si3'
_chemical_formula_weight         447.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.19(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.306(8)
_cell_length_b                   16.0717(7)
_cell_length_c                   19.428(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     5362(3)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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\2q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1365
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6471
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.36
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            maroon
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         6471
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.2174
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.2417
_reflns_number_gt                2039
_reflns_number_total             6471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002743j.txt
_cod_data_source_block           3a
_cod_original_cell_volume        5362(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009689