Cyclic Alumosiloxanes and Alumosilicates: Exemplifying the Loewenstein Rule at the Molecular Level
Sandra González-Gallardo; Vojtech Jancik; Alma A. Delgado-Robles; Mónica Moya-Cabrera; Inorganic Chemistry 50 (2011) 4226–4228; doi:10.1021/ic200313k

data_4325088
_publ_section_title
;
 Cyclic Alumosiloxanes and Alumosilicates: Exemplifying the Loewenstein
 Rule at the Molecular Level
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4226
_journal_page_last               4228
_journal_paper_doi               10.1021/ic200313k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C62 H94 Al2 N4 O8 Si2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C64 H98 Al2 N4 O8.5 Si2'
_chemical_formula_weight         1169.60
_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                 95.57(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.535(2)
_cell_length_b                   25.266(3)
_cell_length_c                   21.606(3)
_cell_measurement_reflns_used    3427
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.30
_cell_volume                     6810.5(17)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12034
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.9379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2007'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         12053
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+4.5157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1407
_reflns_number_gt                8845
_reflns_number_total             12034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200313k_si_002_2.cif
_cod_data_source_block           Compound4
_cod_original_formula_sum        'C64 H98 Al2 N4 O8.50 Si2'
_cod_database_code               4325088