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_4335172
_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         'C53 H97 Al N4 O8 Si2 Zr'
_chemical_formula_sum            'C53 H97 Al N4 O8 Si2 Zr'
_chemical_formula_weight         1092.73
_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                 91.8810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4257(4)
_cell_length_b                   13.0671(5)
_cell_length_c                   37.4401(13)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.26
_cell_volume                     6075.8(4)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            53465
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.9212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       prism
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         10754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0266P)^2^+5.5234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                9534
_reflns_number_total             10754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400156n_si_002_03.cif
_cod_data_source_block           Compound3
_cod_database_code               4335172