Precursors for pyromellit-bridged silica sol‒gel hybrid materials
Pfeifer, Stefan; Schwarzer, Anke; Schmidt, Dana; Brendler, Erica; Veith, Michael; Kroke, Edwin; New Journal of Chemistry 37 (2013) 169–; doi:10.1039/c2nj40538e

data_7052976
_publ_section_title
;
 Precursors for pyromellit-bridged silica sol--gel hybrid materials
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              169
_journal_paper_doi               10.1039/c2nj40538e
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C24 H36 N2 O10 Si2'
_chemical_formula_sum            'C24 H36 N2 O10 Si2'
_chemical_formula_weight         568.73
_chemical_name_common
;
2,6-bis((triethoxysilyl)methyl)pyrrolo(3,4-f) isoindole-1,3,5,7(2H,6H)-tetraone
;
_chemical_name_systematic
;
2,6-bis((triethoxysilyl)methyl)pyrrolo[3,4-f]
isoindole-1,3,5,7(2H,6H)-tetraone
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 99.546(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2971(4)
_cell_length_b                   7.7793(3)
_cell_length_c                   25.6231(7)
_cell_measurement_reflns_used    41553
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      1.44
_cell_volume                     2810.38(16)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 358 frames, detector distance = 120 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36889
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.98
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+1.9990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                4634
_reflns_number_total             5229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40538e.txt
_cod_data_source_block           stpf03_001
_cod_original_cell_volume        2810.38(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052976