Niobium and Zirconium Complexes Incorporating Asymmetrically SubstitutedansaLigands. X-ray Crystal Structures of [Me2Si(η5-C5Me4)(η5-C5H3R)]Nb(NtBu)Cl (R = Me,iPr) and [Me2Si(η5-C5Me4)(η5-C5H3R)]ZrCl2(R = H, Me)
Antiñolo, Antonio; López-Solera, Isabel; Orive, Irache; Otero, Antonio; Prashar, Sanjiv; Rodríguez, Ana M.; Villaseñor, Elena; Organometallics 20 (2001) 71–; doi:10.1021/om0006662

data_4077201
_publ_section_title
;
 Niobium and Zirconium Complexes Incorporating Asymmetrically
 SubstitutedansaLigands. X-ray Crystal Structures of
 [Me2Si(\h5-C5Me4)(\h5-C5H3R)]Nb(NtBu)Cl (R = Me,iPr) and
 [Me2Si(\h5-C5Me4)(\h5-C5H3R)]ZrCl2(R = H, Me)
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              71
_journal_paper_doi               10.1021/om0006662
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C23 H37 Cl N Nb Si'
_chemical_formula_weight         483.99
_chemical_name_systematic
; 
 ? 
;
_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                 110.52(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1550(10)
_cell_length_b                   14.5800(10)
_cell_length_c                   14.8570(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200(2)
_cell_volume                     2465.9(4)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(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\q scans'
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6150
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.653
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+1.6532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                4768
_reflns_number_total             5925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0006662.cif
_cod_data_source_block           12
_cod_original_cell_volume        2465.9(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077201