Synthesis of the Titanium Compound [(MeC5H4)TiCl(μ-NSiMe3)]2 with Migration of a SiMe3 Group and Preparation of Cp2ZrCl(η2-NHNCHSiMe3}
Guangcai Bai; Herbert W. Roesky; Haijun Hao; Mathias Noltemeyer; Hans-Georg Schmidt; Inorganic Chemistry 40 (2001) 2424–2426; doi:10.1021/ic010007x

data_4319645
_publ_contact_author
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       Herbert W. Roesky
       Institut f\"ur Anorganische Chemie
       Universit\"at G\"ottingen
       Tammannstr. 4
       37077 G\"ottingen
       Germany
;
_publ_contact_author_email       hhao@gwdg.de
_publ_contact_author_fax         '049 551 393373'
_publ_contact_author_phone       '049 551 393001'
_publ_section_title
;
 Synthesis of the Titanium Compound [(MeC5H4)TiCl(\m-NSiMe3)]2 with
 Migration of a SiMe3 Group and Preparation of Cp2ZrCl(\h2-NHNCHSiMe3}
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2424
_journal_page_last               2426
_journal_paper_doi               10.1021/ic010007x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C18 H32 Cl2 N2 Si2 Ti2'
_chemical_formula_weight         499.34
_chemical_name_systematic
;
  copmpound 1
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4571(15)
_cell_length_b                   13.4571(15)
_cell_length_c                   13.724(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2485.3(5)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'STOE AED2 four circle diffraktometer'
_diffrn_measurement_method       'profile fitted theta omega scans'
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3699
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         3.66
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.960
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.123
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_obs          0.0304
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.5598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0804
_refine_ls_wR_factor_obs         0.0779
_reflns_number_observed          1589
_reflns_number_total             1622
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010007x_1.cif
_cod_data_source_block           roe724
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.5598P] 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^)+(0.0534P)^2^+0.5598P] 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        2485.4(6)
_cod_database_code               4319645