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_4331755
_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            'C16 H48 O2 Si7 Ti'
_chemical_formula_weight         517.07
_chemical_melting_point          391
_chemical_name_systematic
; 
 \h^2^-[1,1,1,3,3,5,5,5-Octamethyl-2,4-bis(trimethylsilyl)pentasilane-
2,4-diolato]-\h^1^-dimethyl-titanium 
 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.403(2)
_cell_angle_beta                 88.393(2)
_cell_angle_gamma                86.560(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0840(3)
_cell_length_b                   10.1608(3)
_cell_length_c                   15.8011(5)
_cell_measurement_reflns_used    8856
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      40.17
_cell_measurement_theta_min      2.22
_cell_volume                     1588.29(8)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44454
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.8413
_exptl_absorpt_correction_T_min  0.6707
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.7620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                5009
_reflns_number_total             5466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0514997sup1.cif
_cod_data_source_block           w76(11)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      'P-1   '
_cod_database_code               4331755