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_7227264
_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_sum            'C80 H88 O30 Si8'
_chemical_formula_weight         1754.22
_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-2014/7
_audit_update_record
;
2016-10-12 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.936(10)
_cell_angle_beta                 76.182(9)
_cell_angle_gamma                78.08(2)
_cell_formula_units_Z            1
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_cell_length_b                   12.114(3)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.677
_cell_measurement_theta_min      1.631
_cell_volume                     1980.6(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'Dectris PILATUS2 6M'
_diffrn_measured_fraction_theta_full 0.800
_diffrn_measured_fraction_theta_max 0.739
_diffrn_measurement_device_type  'ESRF-EMBL  MD2M diffractometer'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'ESRF synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8729
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.800
_diffrn_reflns_Laue_measured_fraction_max 0.739
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19447
_diffrn_reflns_point_group_measured_fraction_full 0.800
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_diffrn_reflns_theta_max         32.677
_diffrn_reflns_theta_min         1.631
_diffrn_source_type              'ID23-2 microfocus'
_exptl_absorpt_coefficient_mu    0.224
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.06
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_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.454
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_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         5795
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_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0586
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1129P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4132
_reflns_number_total             5795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02369j2.cif
_cod_data_source_block           dv202
_cod_depositor_comments
'Adding full bibliography for 7227263--7227264.cif.'
_cod_database_code               7227264
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              6123