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_4335177
_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 Al2 N4 O16 Si4 Zr, 2.88(C7 H8)'
_chemical_formula_sum            'C110.16 H177.04 Al2 N4 O16 Si4 Zr'
_chemical_formula_weight         2071.06
_chemical_name_systematic
;
 ?
;
_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                 90.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.768(2)
_cell_length_b                   46.784(5)
_cell_length_c                   19.654(3)
_cell_measurement_reflns_used    9221
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.25
_cell_volume                     11740(3)
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77646
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2008 Sheldrick'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       prism
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.446
_exptl_crystal_size_min          0.348
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1609
_refine_ls_number_reflns         20695
_refine_ls_number_restraints     1568
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0559P)^2^+17.8953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                17023
_reflns_number_total             20695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400156n_si_002_08.cif
_cod_data_source_block           Compound8
_cod_database_code               4335177