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_7010167
_publ_section_title
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 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;
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_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_formula_moiety         'C36 H68 N8 Si4 Zr2'
_chemical_formula_sum            'C36 H68 N8 Si4 Zr2'
_chemical_formula_weight         907.78
_chemical_name_common            '[{Zr(C6H4(NSiMe2vinyl)2)(NMe2)2}2]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.00(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.596(11)
_cell_length_b                   10.248(4)
_cell_length_c                   25.869(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     4602(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scan'
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6614
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         3.147
_refine_diff_density_min         -2.101
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_obs          0.0704
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1522P)^2^+5.3904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1995
_refine_ls_wR_factor_obs         0.1918
_reflns_number_observed          5776
_reflns_number_total             6398
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006596j.txt
_cod_data_source_block           jun397-MFL4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1522P)^2^+5.3904P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1522P)^2^+5.3904P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4602.5(40)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010167