Control of micro/mesoporosity in non-hydrolytic hybrid silicophosphate xerogels
Styskalik, Ales; Skoda, David; Moravec, Zdenek; Babiak, Michal; Barnes, Craig E.; Pinkas, Jiri; Journal of Materials Chemistry A 3 (2015) 7477–; doi:10.1039/C4TA06823H

data_7235845
_publ_section_title
;
 Control of micro/mesoporosity in non-hydrolytic hybrid silicophosphate
 xerogels
;
_journal_issue                   14
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              7477
_journal_paper_doi               10.1039/C4TA06823H
_journal_volume                  3
_journal_year                    2015
_chemical_formula_sum            'C37 H48 O8 P2 Si4'
_chemical_formula_weight         795.05
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2014-12-11 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.200(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2590(3)
_cell_length_b                   11.6835(3)
_cell_length_c                   16.8330(4)
_cell_measurement_reflns_used    5192
_cell_measurement_temperature    120(2)
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_cell_measurement_theta_min      3.0740
_cell_volume                     2016.13(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7506
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         3.488
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'Mon May 07 21:37:24 2012' 
;
_exptl_crystal_colour            coulourless
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane and THF 10:2 v/v'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.373
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_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3682
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0565P)^2^+0.0488P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                3049
_reflns_number_total             3682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ta06823h2.cif
_cod_data_source_block           Ales1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7235845
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.922
_shelxl_version_number           2013-2
_shelx_res_checksum              87361