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_7123761
_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(C30 H25 B O7 Si4)'
_chemical_formula_sum            'C60 H50 B2 O14 Si8'
_chemical_formula_weight         1241.34
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1z6vpq
_audit_creation_date             2018-02-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5467)
;
_audit_update_record
;
2018-02-13 deposited with the CCDC.    2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.7490(10)
_cell_angle_beta                 78.4840(10)
_cell_angle_gamma                68.2650(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0387(9)
_cell_length_b                   13.2083(9)
_cell_length_c                   19.4033(14)
_cell_measurement_reflns_used    7265
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.46
_cell_volume                     2997.0(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0862
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29082
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.386
_diffrn_reflns_theta_min         1.684
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0653 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.9097. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       hexagonal_plate
_exptl_crystal_F_000             1288
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0791P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6867
_reflns_number_total             10990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03972d2.cif
_cod_data_source_block           rem218a
_cod_database_code               7123761
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C52A) = Uanis(C50A)
Uanis(C50) = Uanis(C53A)
Uanis(C51) = Uanis(C51A)
3. Others
 Fixed Sof: C50(0.5) H50(0.5) C50A(0.5) H50A(0.5) C51(0.5) H51(0.5) C51A(0.5)
 H51A(0.5) C52(0.5) H52(0.5) C52A(0.5) H52A(0.5) C53(0.5) H53(0.5) C53A(0.5)
 H53A(0.5) C54(0.5) H54(0.5) C54A(0.5) H54A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C50A(H50A), C51(H51), C51A(H51A), C52(H52), C52A(H52A),
 C53(H53), C53A(H53A), C54(H54), C54A(H54A), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60)
;
_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 'RM PhBT8PhB'
_olex2_submission_special_instructions 'No special instructions were received'