Fluorinated Diarylamido Complexes of Lithium, Zirconium, and Hafnium
Wei-Ying Lee; Lan-Chang Liang; Inorganic Chemistry 47 (2008) 3298–3306; doi:10.1021/ic702293d

data_4304725
_publ_section_title
;
Fluorinated Diarylamido Complexes of Lithium, Zirconium, and Hafnium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3298
_journal_page_last               3306
_journal_paper_doi               10.1021/ic702293d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C40 H52 Cl2 F2 N2 O Zr'
_chemical_formula_sum            'C40 H52 Cl2 F2 N2 O Zr'
_chemical_formula_weight         776.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.6730(10)
_cell_angle_beta                 86.7590(10)
_cell_angle_gamma                68.3530(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4422(2)
_cell_length_b                   13.03410(10)
_cell_length_c                   14.8695(2)
_cell_measurement_reflns_used    37728
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_volume                     2011.15(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30725
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.9428
_exptl_absorpt_correction_T_min  0.7413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0137(12)
_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   1.126
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0645P)^2^+0.7126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                7865
_reflns_number_total             9209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702293d-file002_2.cif
_cod_data_source_block           6456
_cod_original_cell_volume        2011.15(4)
_cod_database_code               4304725