Bis{4,4',6,6'-tetrachloro-2,2'-[<i>trans</i>-(<i>R</i>,<i>R</i>)-cyclohexane-1,2-diylbis(iminomethylene)]diphenolato-κ^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}zirconium(IV)
Shalumova, Tamila; Tanski, Joseph M.; Acta Crystallographica Section E 64 (2008) m1029–m1030; doi:10.1107/S1600536808021247

data_2219159
_publ_section_title
Bis{4,4',6,6'-tetrachloro-2,2'-[<i>trans</i>-(<i>R</i>,<i>R</i>)-cyclohexane-1,2-diylbis(iminomethylene)]diphenolato-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}zirconium(IV)
_journal_coeditor_code           RZ2233
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1029
_journal_page_last               m1030
_journal_paper_doi               10.1107/S1600536808021247
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zr (C20 H20 Cl4 N2 O2)2]'
_chemical_formula_moiety         'C40 H40 Cl8 N4 O4 Zr'
_chemical_formula_sum            'C40 H40 Cl8 N4 O4 Zr'
_chemical_formula_weight         1015.58
_chemical_name_systematic
;
Bis{4,4',6,6'-tetrachloro-2,2'-[<i>trans</i>-(R,R)-cyclohexane-1,2-
diylbis(iminomethylene)]diphenolato-\k^4^O,N,N',O'}zirconium(IV)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 114.6860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2570(6)
_cell_length_b                   16.4848(8)
_cell_length_c                   12.7431(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.34
_cell_volume                     2148.62(19)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29336
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.373
_refine_ls_abs_structure_details 'Flack (1983), 5344 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         11081
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.024P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                9280
_reflns_number_total             11081
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2233.cif
_cod_data_source_block           I
_cod_original_cell_volume        2148.62(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2219159
_cod_database_fobs_code          2219159