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_4077200
_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            'C21 H33 Cl N Nb Si'
_chemical_formula_weight         455.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6810(10)
_cell_length_b                   17.0030(10)
_cell_length_c                   17.0590(10)
_cell_measurement_temperature    200(2)
_cell_volume                     4548.3(5)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harm, 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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11441
_diffrn_reflns_theta_full        27.82
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.703
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         10750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0480P)^2^+4.3387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                8170
_reflns_number_total             10750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0006662.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4077200