Bis[(1<i>R</i>,2<i>R</i>)-({-})-1,2-bis(trimethylsilylamino)cyclohexane(2{-})-κ^2^<i>N,N</i>']zirconium(IV)
Jian-Feng Li; Lin-Hong Weng; Shu-Ping Huang; Hong-Bo Tong; Dian-Sheng Liu; Acta Crystallographica Section E 58 (2002) m510–m512; doi:10.1107/S1600536802015660

data_2201231
_publ_section_title
Bis[(1<i>R</i>,2<i>R</i>)-({-})-1,2-bis(trimethylsilylamino)cyclohexane(2{-})-\k^2^<i>N,N</i>']zirconium(IV)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m510
_journal_page_last               m512
_journal_paper_doi               10.1107/S1600536802015660
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Zr (C12 H28 N2 Si2)2]'
_chemical_formula_moiety         'C24 H56 N4 Si4 Zr'
_chemical_formula_sum            'C24 H56 N4 Si4 Zr'
_chemical_formula_weight         604.31
_chemical_name_systematic
;
bis[(1R,2R)-(-)-1,2-bis(trimethylsilylamino)cyclohexane-\k^2^N,N']zirconium
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.473(5)
_cell_length_b                   10.473(5)
_cell_length_c                   28.166(18)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.002
_cell_measurement_theta_min      2.245
_cell_volume                     2675(2)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            11157
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        4.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_correction_T_min  0.8557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.483
_refine_diff_density_min         -1.042
_refine_ls_abs_structure_details 'Flack (1983), 0000 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.281
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0337P)^2^+2.5967P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                4526
_reflns_number_total             4626
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac6011.cif
_cod_data_source_block           I
_cod_original_cell_volume        2676(2)
_cod_database_code               2201231
_cod_database_fobs_code          2201231