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_7123762
_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 O7 Si4)'
_chemical_formula_sum            'C62 H54 B2 O14 Si8'
_chemical_formula_weight         1269.39
_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     direct
_audit_creation_date             2018-06-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-19 deposited with the CCDC.    2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                76.1452(8)
_cell_angle_beta                 76.4917(10)
_cell_angle_gamma                69.0621(9)
_cell_formula_units_Z            2
_cell_length_a                   13.2208(2)
_cell_length_b                   13.2988(2)
_cell_length_c                   19.7225(3)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.82
_cell_measurement_theta_min      2.34
_cell_volume                     3102.25(8)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXT (Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.36
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.929
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29282
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.996
_diffrn_reflns_theta_min         2.339
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0484 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.8924. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       cube
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         11139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0504P)^2^+0.8634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9463
_reflns_number_total             11139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03972d2.cif
_cod_data_source_block           rem618a
_cod_original_cell_volume        3102.26(8)
_cod_database_code               7123762
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.692
_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. Others
 Fixed Sof: C46(0.5) H46(0.5) C46A(0.5) H46A(0.5) C47(0.5) H47(0.5) C47A(0.5)
 H47A(0.5) C48(0.5) H48(0.5) C48A(0.5) H48A(0.5) C49(0.5) H49(0.5) C49A(0.5)
 H49A(0.5) C50(0.5) H50(0.5) C50A(0.5) H50A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42),
  C43(H43), C44(H44), C46(H46), C46A(H46A), C47(H47), C47A(H47A), C48(H48),
 C48A(H48A), C49(H49), C49A(H49A), C50(H50), C50A(H50A), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              88190
_contact_crystallographer_email  xraystaples@crystalspec.com
_contact_crystallographer_name   'Richard Staples'
_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-AA#9
_olex2_submission_special_instructions 'No special instructions were received'