A General Diversity Oriented Synthesis of Asymmetric Double-Decker Shaped Silsesquioxanes
Barry, Badru-Deen; Dannatt, Jonathan Elvin; King, Austin Kendall; Lee, Andre; Maleczka, Robert; Chemical Communications  (2019) –; doi:10.1039/C9CC03972D

data_7123763
_publ_section_title
;
 A General Diversity Oriented Synthesis of Asymmetric Double-Decker Shaped
 Silsesquioxanes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03972D
_journal_year                    2019
_chemical_formula_moiety         '2(C31 H27 B O8 Si4)'
_chemical_formula_sum            'C62 H54 B2 O16 Si8'
_chemical_formula_weight         1301.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1zw0mh
_audit_creation_date             2018-05-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-14 deposited with the CCDC.    2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7461(3)
_cell_length_b                   22.7525(4)
_cell_length_c                   11.4396(2)
_cell_measurement_reflns_used    4758
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.73
_cell_measurement_theta_min      3.58
_cell_volume                     6428.01(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1278
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44545
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.196
_diffrn_reflns_theta_min         1.789
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.135
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0823 before and 0.0662 after correction. The Ratio of minimum to maximum transmission is 0.7842. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         12430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7168
_reflns_number_total             12430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03972d2.cif
_cod_data_source_block           rem518a
_cod_database_code               7123763
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C9A(H9A), C10A(H10A), C11A(H11A),
 C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A),
 C19A(H19A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A),
 C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A), C2B(H2B), C3B(H3B),
  C5B(H5B), C6B(H6B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C13B(H13B),
 C15B(H15B), C016(H016), C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B),
 C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B), C26B(H26B), C27B(H27B),
 C28B(H28B), C29B(H29B), C30B(H30B)
2.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id 'REM 5 -3 -2018'
_olex2_submission_special_instructions 'No special instructions were received'