Synthesis, structures and catalytic properties of chelating N,N '-bis(silylated) 1,2-benzenediamidozirconium(IV) chlorides [and a titanium(IV) analogue] and dimethylamides †
Danièle, Stephane; Hitchcock, Peter B.; Lappert, Michael F.; Merle, Philippe G.; Journal of the Chemical Society, Dalton Transactions  (2001) 13–; doi:10.1039/b006596j

data_7010169
_publ_section_title
;
 Synthesis, structures and catalytic properties of chelating
 N,N&#x200A;'-bis(silylated) 1,2-benzenediamidozirconium(IV) chlorides
 [and a titanium(IV) analogue] and dimethylamides&#x200A;&#x2020;
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              13
_journal_paper_doi               10.1039/b006596j
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H68 N8 Si4 Zr2'
_chemical_formula_structural     'C32 H68 N8 Si4 Zr2'
_chemical_formula_sum            'C32 H68 N8 Si4 Zr2'
_chemical_formula_weight         859.74
_chemical_name_common            '[{Zr(NMe2)2(C6H4(NSiMe3)2)}2]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-10-27T09:52:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.8770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7431(4)
_cell_length_b                   10.1941(2)
_cell_length_c                   18.7501(4)
_cell_measurement_reflns_used    12797
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     4389.02(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23086
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         4.32
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9039
_exptl_absorpt_correction_T_min  0.8325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00096(13)
_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   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+4.9560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                4722
_reflns_number_total             5216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006596j.txt
_cod_data_source_block           oct2999-MFL7
_cod_original_cell_volume        4389.02(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010169