Homo- and heteroalumoxane silicates
García-Ríos, Jessica; Hernández-Campos, René Francisco; Rascón-Cruz, Fernando; Moreno-Martínez, Víctor Augusto; Huerta-Lavorie, Raúl; Velázquez-Carmona, Miguel-Ángel; Cea-Olivares, Raymundo; Martínez-Otero, Diego; Jancik, Vojtech; RSC Advances 5 (2015) 99722–; doi:10.1039/C5RA18481A

data_7235993
_publ_section_title
;
 Homo- and heteroalumoxane silicates
;
_journal_issue                   121
_journal_name_full               'RSC Advances'
_journal_page_first              99722
_journal_paper_doi               10.1039/C5RA18481A
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C76 H124 Al2 N4 O10 Si2 Zn3, 0.84(C4 H8 O)'
_chemical_formula_sum            'C79.36 H130.72 Al2 N4 O10.84 Si2 Zn3'
_chemical_formula_weight         1620.60
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-25 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.51(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3480(10)
_cell_length_b                   22.490(2)
_cell_length_c                   16.843(2)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.52
_cell_volume                     4380.9(9)
_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, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48084
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.361
_diffrn_reflns_theta_min         1.577
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_correction_T_min  0.7518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2007'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1731
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.394(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         15961
_refine_ls_number_restraints     592
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                12991
_reflns_number_total             15961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra18481a2.cif
_cod_data_source_block           Comp9
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7235993
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.892
_shelx_res_checksum              8678