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_4331753
_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            'C22 H58 Cl2 O4 Si7 Zr'
_chemical_formula_weight         745.43
_chemical_melting_point          467
_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- \h^1^-bis(tetrahydrofuranato)-zirconium 
 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.5240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4226(2)
_cell_length_b                   22.8237(4)
_cell_length_c                   17.9217(3)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.09
_cell_measurement_theta_min      2.06
_cell_volume                     4107.72(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51845
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.8748
_exptl_absorpt_correction_T_min  0.7056
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+4.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                6576
_reflns_number_total             7225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0514997sup1.cif
_cod_data_source_block           w39a(9)
_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)/n  '
_cod_database_code               4331753