Synthesis and characterization of highly pure azido-functionalized polyhedral oligomeric silsesquioxanes (POSS)
Vuthichai Ervithayasuporn; Xin Wang; Yusuke Kawakami; Chem. Commun. 34 (2009) 5130–5132; doi:10.1039/b909802j

data_7104693
_publ_section_title
;
 Synthesis and characterization of highly pure azido-functionalized
 polyhedral oligomeric silsesquioxanes (POSS)
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              5130
_journal_page_last               5132
_journal_paper_doi               10.1039/b909802j
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C56 H58 N6 O14 Si10 '
_chemical_formula_sum            'C56 H58 N6 O14 Si10'
_chemical_formula_weight         1319.96
_chemical_name_common
;
trans-3,13-di(3-azidopropyl)-3,13-dimethyl-
1,5,7,9,11,15,17,19-
octaphenylhexacyclo(15.3.1(1,13).1(3,11).1(5,17).1(9,15))decasiloxane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                68.2520(13)
_cell_angle_beta                 71.0568(13)
_cell_angle_gamma                68.8461(13)
_cell_formula_units_Z            1
_cell_length_a                   9.9231(2)
_cell_length_b                   13.2854(3)
_cell_length_c                   13.9868(7)
_cell_measurement_reflns_used    16962
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.4
_cell_measurement_theta_min      3.5
_cell_volume                     1557.98(9)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17649
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5487
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0654P)^2^+4.3303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1652
_reflns_number_gt                4874
_reflns_number_total             5487
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b909802j.txt
_cod_data_source_block           '_DDQ-N3'
_cod_original_formula_sum        'C56 H58 N6 O14 Si10 '
_cod_database_code               7104693