Heterometallic Alumo- and Gallodisilicates with M(O-Si-O)2M' and [M(O-Si-O)2]2M' Cores (M = Al, Ga; M' = Ti, Zr, Hf)
Raúl Huerta-Lavorie; Diego Solis-Ibarra; Dana Victoria Báez-Rodríguez; Marisol Reyes-Lezama; M. de las Nieves Zavala-Segovia; Vojtech Jancik; Inorganic Chemistry 52 (2013) 6934–6943; doi:10.1021/ic400156n

data_4335180
_publ_section_title
;
 Heterometallic Alumo- and Gallodisilicates with M(O-Si-O)2M' and
 [M(O-Si-O)2]2M' Cores (M = Al, Ga; M' = Ti, Zr, Hf)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6934
_journal_page_last               6943
_journal_paper_doi               10.1021/ic400156n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C90 H154 Ga2 Hf N4 O16 Si4, 1.378(C6H14), 0.122(C7H8)'
_chemical_formula_sum            'C99.12 H174.26 Ga2 Hf N4 O16 Si4'
_chemical_formula_weight         2108.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.2160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8092(9)
_cell_length_b                   33.807(2)
_cell_length_c                   24.3049(15)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      2.22
_cell_volume                     11130.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            120025
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.8162
_exptl_absorpt_correction_T_min  0.5718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick 2008/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             4460
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1380
_refine_ls_number_reflns         19707
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+43.2950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                16822
_reflns_number_total             19707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400156n_si_002_11.cif
_cod_data_source_block           Compound11
_cod_original_cell_volume        11130.1(12)
_cod_database_code               4335180