Addition and Metathesis Reactions of Zirconium and Hafnium Imido Complexes
Joseph L. Thorman; Ilia A. Guzei; Victor G. Young,; L. Keith Woo; Inorganic Chemistry 39 (2000) 2344–2351; doi:10.1021/ic9910007

data_4320969
_publ_section_title
;
 Addition and Metathesis Reactions of Zirconium and Hafnium Imido
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2344
_journal_page_last               2351
_journal_paper_doi               10.1021/ic9910007
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C76.5 H84 N4 O2 Zr'
_chemical_formula_weight         1182.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.6240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8318(8)
_cell_length_b                   20.7139(8)
_cell_length_c                   15.7878(8)
_cell_measurement_temperature    173(2)
_cell_volume                     6590.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7601
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.9383
_exptl_absorpt_correction_T_min  0.9383
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7601
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.698
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1509P)^2^+5.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2084
_reflns_number_gt                6076
_reflns_number_total             7601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9910007_2.cif
_cod_data_source_block           woo03
_cod_original_formula_sum        'C76.50 H84 N4 O2 Zr'
_cod_database_code               4320969