Unusual cis and trans architecture of dihydrofunctional double-decker shaped silsesquioxane and synthesis of its ethyl bridged π-conjugated arene derivatives
Walczak, M.; Januszewski, R.; Majchrzak, M.; Kubicki, M.; Dudziec, B.; Marciniec, B.; New J. Chem. 41 (2017) 3290–; doi:10.1039/C7NJ00255F

data_7056154
_publ_section_title
;
 Unusual cis and trans architecture of dihydrofunctional double-decker
 shaped silsesquioxane and synthesis of its ethyl bridged \p-conjugated
 arene derivatives
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              3290
_journal_paper_doi               10.1039/C7NJ00255F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C50 H46 O14 Si10'
_chemical_formula_sum            'C50 H46 O14 Si10'
_chemical_formula_weight         1151.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-05-23 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                98.402(4)
_cell_angle_beta                 90.407(3)
_cell_angle_gamma                90.950(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5118(5)
_cell_length_b                   13.8528(8)
_cell_length_c                   19.5175(6)
_cell_measurement_reflns_used    6786
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      27.5090
_cell_measurement_theta_min      3.3090
_cell_volume                     2811.1(2)
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_collection       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_molecular_graphics    'Mercury (MacRae, 2007)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      130(1)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19356
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.079
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7282
_reflns_number_total             9894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00255f2.cif
_cod_data_source_block           1
_cod_database_code               7056154
_shelxl_version_number           2013-4
_shelx_res_checksum              96827