The First Niobasilsesquioxanes§
Lorenz, Volker; Blaurock, Steffen; Görls, Helmar; Edelmann, Frank T.; Organometallics 25 (2006) 5922–; doi:10.1021/om0606587

data_4074457
_publ_section_title
;
 The First Niobasilsesquioxanes&#x00A7;
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5922
_journal_paper_doi               10.1021/om0606587
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C52 H100 Nb2 O18 Si6'
_chemical_formula_weight         1367.68
_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                104.56(3)
_cell_angle_beta                 96.05(3)
_cell_angle_gamma                108.18(3)
_cell_formula_units_Z            2
_cell_length_a                   14.677(3)
_cell_length_b                   14.949(3)
_cell_length_c                   17.199(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      3.52
_cell_volume                     3400.0(15)
_computing_cell_refinement       'Stoe XAREA'
_computing_data_collection       'Stoe XAREA'
_computing_data_reduction        'Stoe XAREA'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       '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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32557
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.8239
_exptl_absorpt_correction_T_min  0.7867
_exptl_absorpt_correction_type   XRED32
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.985
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         20258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0568
_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^)+(0.1157P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                14264
_reflns_number_total             20258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0606587si20060721_054038.cif
_cod_data_source_block           st116a
_cod_original_cell_volume        3399.9(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074457