Trisilane-1,3-diolato Complexes of Ti and Zr: Syntheses and X-ray Crystal Structures†
Krempner, C.; Köckerling, M.; Reinke, H.; Weichert, K.; Inorganic Chemistry 45 (2006) 3203–3211; doi:10.1021/ic0514997

data_4331752
_publ_section_title
;
 Trisilane-1,3-diolato Complexes of Ti and Zr:&#x00A0; Syntheses and X-ray
 Crystal Structures&#x2020;
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3203
_journal_page_last               3211
_journal_paper_doi               10.1021/ic0514997
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C14 H42 Cl2 O2 Si7 Ti'
_chemical_formula_weight         557.91
_chemical_melting_point          406
_chemical_name_systematic
; 
 \h^2^-[1,1,1,3,3,5,5,5-Octamethyl-2,4-bis(trimethylsilyl)pentasilane-
2,4-diolato]-\h^1^-dichloro-titanium 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.2210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3300(2)
_cell_length_b                   17.7010(4)
_cell_length_c                   9.9319(2)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      37.45
_cell_measurement_theta_min      2.97
_cell_volume                     1608.90(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8Apex CCD'
_diffrn_measurement_method       'phi and 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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            85555
_diffrn_reflns_theta_full        40.00
_diffrn_reflns_theta_max         40.00
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.8443
_exptl_absorpt_correction_T_min  0.6991
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         19735
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.0089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                16599
_reflns_number_total             19735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0514997sup1.cif
_cod_data_source_block           w40(7)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_database_code               4331752