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_4077203
_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            'C8.5 H11.5 Cl Si0.5 Zr0.5'
_chemical_formula_weight         208.78
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   10.626(8)
_cell_length_b                   13.839(3)
_cell_length_c                   12.470(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    250(2)
_cell_volume                     1833.8(19)
_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 0.996
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.4883
_diffrn_reflns_av_sigmaI/netI    0.2850
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2993
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0011(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.3153
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.2625
_reflns_number_gt                490
_reflns_number_total             2293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0006662.cif
_cod_data_source_block           14
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C8.50 H11.50 Cl Si0.50 Zr0.50'
_cod_database_code               4077203