Synthesis and Structures of Titanium and Zirconium Trisiloxides
Krempner, Clemens; Jäger-Fiedler, Ulrike; Köckerling, Martin; Reinke, Helmut; Organometallics 28 (2009) 382–; doi:10.1021/om800930s

data_4068547
_publ_section_title
;
 Synthesis and Structures of Titanium and Zirconium Trisiloxides
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              382
_journal_paper_doi               10.1021/om800930s
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C50 H150 O7 Si26 Ti2'
_chemical_formula_sum            'C50 H150 O7 Si26 Ti2'
_chemical_formula_weight         1689.84
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'ct.exe (M. K\"ockerling, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 117.60(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.47(2)
_cell_length_b                   25.00(1)
_cell_length_c                   16.228(9)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.407
_cell_measurement_theta_min      3.403
_cell_volume                     10955(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.559
_diffrn_measured_fraction_theta_max 0.559
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5015
_diffrn_reflns_theta_full        23.02
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.463
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                2415
_reflns_number_total             4276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800930s_si_001.cif
_cod_data_source_block           KR357-Si26C50H150O7Ti2
_cod_original_cell_volume        10955(10)
_cod_database_code               4068547