Molecular Gallosilicates and Their Group 4 Multimetallic Derivatives
Diego Solis-Ibarra; Miriam Velásquez-Hernández; Raúl Huerta-Lavorie; Vojtech Jancik; Inorganic Chemistry 50 (2011) 8907–8917; doi:10.1021/ic200976d

data_4326236
_publ_section_title
;
 Molecular Gallosilicates and Their Group 4 Multimetallic Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8907
_journal_page_last               8917
_journal_paper_doi               10.1021/ic200976d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C76 H125 Ga2 N5 O10 Si2 Zr, C6 H14'
_chemical_formula_sum            'C82 H139 Ga2 N5 O10 Si2 Zr'
_chemical_formula_weight         1641.82
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.759(2)
_cell_length_b                   17.415(2)
_cell_length_c                   28.487(3)
_cell_measurement_reflns_used    7782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.64
_cell_volume                     8807.3(17)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.34A, Bruker 2006)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.34A, Bruker 2006)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23499
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.8376
_exptl_absorpt_correction_T_min  0.7591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         7978
_refine_ls_number_restraints     1325
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.8337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                5845
_reflns_number_total             7978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200976d_si_002_10.cif
_cod_data_source_block           Compound9_NHMe2
_cod_database_code               4326236