Eight Membered Cyclic-Borasiloxanes: Synthesis, Structural, Photophysical, Steric Strain and DFT calculations
Mohan, Gopalakrishnan; Thirumoorthy, Krishnan; Bhuvanesh, Nattamai; Nallasamy, Palanisami; RSC Adv.  (2016) –; doi:10.1039/C6RA02080A

data_7225391
_publ_section_title
;
 Eight Membered Cyclic-Borasiloxanes: Synthesis, Structural,
 Photophysical, Steric Strain and DFT calculations
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA02080A
_journal_year                    2016
_chemical_formula_moiety         '2(C24 H19 B O2 Si)'
_chemical_formula_sum            'C48 H38 B2 O4 Si2'
_chemical_formula_weight         756.58
_chemical_name_systematic
'4,8-di([1,1'-biphenyl]-2-yl)-2,2,6,6-tetraphenyl-1,3,5,7,2,6,4,8-tetraoxadisiladiborocane '
_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_date             2014-12-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2015-02-03 deposited with the CCDC.
2016-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                102.339(3)
_cell_angle_beta                 92.109(3)
_cell_angle_gamma                100.314(3)
_cell_formula_units_Z            2
_cell_length_a                   9.918(2)
_cell_length_b                   12.032(3)
_cell_length_c                   17.307(4)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.454
_cell_measurement_theta_min      2.334
_cell_volume                     1978.9(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22817
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         1.765
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1515 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.5821.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.069
_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     505
_refine_ls_number_reflns         8908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0571P)^2^+0.7957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7204
_reflns_number_total             8908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra02080a2.cif
_cod_data_source_block           gp46
_cod_database_code               7225391
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C2(H2), C12A(H12A), C23A(H23A), C2A(H2A), C11A(H11A), C20A(H20A),
 C14A(H14A), C5A(H5A), C21A(H21A), C18A(H18A), C3A(H3A), C24(H24), C22A(H22A),
 C8A(H8A), C20(H20), C5(H5), C3(H3), C17A(H17A), C18(H18), C14(H14), C10A(H10A),
  C4(H4), C15A(H15A), C12(H12), C8(H8), C9A(H9A), C4A(H4A), C16A(H16A),
 C23(H23), C17(H17), C21(H21), C15(H15), C16(H16), C11(H11), C10(H10), C9(H9),
 C22(H22)
;
_shelx_res_checksum              97347
_olex2_submission_special_instructions 'No special instructions were received'