Hydrogen bond-directed assembly of silsesquioxanes cubes: synthesis of carboxylic acid POSS derivatives and the solid state structure of octa[2-(p-carboxyphenyl)ethyl] silsesquioxane
Voisin, Doria; Flot, David; Van der Lee, Arie; Dautel, Olivier J.; Moreau, Joel J. E.; CrystEngComm 19 (2017) 492–; doi:10.1039/C6CE02369J

data_7227263
_publ_section_title
;
 Hydrogen bond-directed assembly of silsesquioxanes cubes: synthesis of
 carboxylic acid POSS derivatives and the solid state structure of
 octa[2-(p-carboxyphenyl)ethyl] silsesquioxane
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              492
_journal_paper_doi               10.1039/C6CE02369J
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C128 H104 O28 Si8'
_chemical_formula_sum            'C128 H104 O28 Si8'
_chemical_formula_weight         2314.84
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_update_record
;
2016-10-05 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                82.048(5)
_cell_angle_beta                 72.999(6)
_cell_angle_gamma                68.508(8)
_cell_formula_units_Z            1
_cell_length_a                   13.7763(12)
_cell_length_b                   16.0926(12)
_cell_length_c                   17.8036(10)
_cell_measurement_reflns_used    5642
_cell_measurement_temperature    175
_cell_measurement_theta_max      27.2570
_cell_measurement_theta_min      1.7510
_cell_volume                     3509.9(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_details
;
  1 omega    1.00   42.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -       13.3138  -77.0000  -90.0000 41

  2 omega  -12.00   21.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9388 -100.0000 -180.0000 33

  3 omega  -42.00   60.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -       13.3138    0.0000 -180.0000 102

  4 omega  -17.00   49.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -       13.3138 -100.0000   30.0000 66

  5 omega  -22.00   23.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9388 -100.0000   60.0000 45

  6 omega  -55.00   32.00   1.0000  175.0000
omega____ theta____ kappa____ phi______ frames
    -       13.3138  -57.0000  150.0000 87

;
_diffrn_measurement_device       Area
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_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_12      0.0196454000
_diffrn_orient_matrix_UB_13      0.0052753000
_diffrn_orient_matrix_UB_21      0.0399989000
_diffrn_orient_matrix_UB_22      -0.0224550000
_diffrn_orient_matrix_UB_23      -0.0330303000
_diffrn_orient_matrix_UB_31      -0.0199711000
_diffrn_orient_matrix_UB_32      0.0368156000
_diffrn_orient_matrix_UB_33      -0.0249158000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
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_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    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
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_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 35.4 35.9 32.5 12.1 
;
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     I>2.0\s(I)
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_oxford_refine_ls_scale          3.165(13)
_oxford_reflns_number_all        10052
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
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_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7227263--7227264.cif.'
_cod_original_cell_volume        3509.9(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7227263
_cell_oxdiff_length_a            13.8058(10)
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_cell_oxdiff_angle_alpha         81.904(4)
_cell_oxdiff_angle_beta          72.758(5)
_cell_oxdiff_angle_gamma         68.535(6)
_cell_oxdiff_volume              3516.6(3)
_montpellier_reflns_maxres       0.88
_montpellier_reflns_completeness_maxres 99.97
_montpellier_reflns_redundancy_maxres 2.11