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_7235989
_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         'C42 H70 Al2 N2 O6 Si'
_chemical_formula_sum            'C42 H70 Al2 N2 O6 Si'
_chemical_formula_weight         781.05
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-25 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3921(3)
_cell_length_b                   17.0679(5)
_cell_length_c                   20.9414(6)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.25
_cell_volume                     4429.3(2)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9224
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.365
_diffrn_reflns_theta_min         1.539
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1, Sheldrick'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Toluene'
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
; 
 Flack x determined using 2836 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9224
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0412P)^2^+0.8686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8125
_reflns_number_total             9224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra18481a2.cif
_cod_data_source_block           Comp4
_cod_database_code               7235989
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2013-4
_shelx_res_checksum              40057