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_7225392
_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(C20 H19 B O2 Si)'
_chemical_formula_sum            'C40 H38 B2 O4 Si2'
_chemical_formula_weight         660.50
_chemical_name_systematic
'4,8-bis(4-ethylphenyl)-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             2014-12-11
_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                86.890(2)
_cell_angle_beta                 82.970(2)
_cell_angle_gamma                83.983(2)
_cell_formula_units_Z            2
_cell_length_a                   9.349(2)
_cell_length_b                   12.040(3)
_cell_length_c                   16.080(3)
_cell_measurement_reflns_used    8798
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.476
_cell_measurement_theta_min      2.205
_cell_volume                     1784.9(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.985
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21066
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         1.702
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0726 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.9270.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.53
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8092
_refine_ls_number_restraints     584
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0538P)^2^+1.1126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6832
_reflns_number_total             8092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra02080a2.cif
_cod_data_source_block           gp47
_cod_original_cell_volume        1785.1(7)
_cod_database_code               7225392
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7B-C4B \\sim C7A-C4A
 with sigma of 0.005
 C8B-C7B \\sim C8A-C7A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A \\sim C15B \\sim
C16B \\sim C17B \\sim C18B \\sim C19B \\sim C20B: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.01
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B:
within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1B) = Uanis(C1A)
4. Rigid body (RIGU) restrains
 C15A, C16A, C17A, C18A, C19A, C20A, C15B, C16B, C17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Others
 Sof(C15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=
 Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=1-FVAR(1)
 Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=FVAR(1)
 Sof(C1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=
 Sof(H8BC)=1-FVAR(2)
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C7A(H7AA,H7AB), C7B(H7BA,H7BB)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C2A(H2A), C3A(H3A),
  C5A(H5A), C6A(H6A), C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C10A(H10A),
 C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A), C16A(H16A), C17A(H17A),
 C18A(H18A), C19A(H19A), C20A(H20A), C16B(H16B), C17B(H17B), C18B(H18B),
 C19B(H19B), C20B(H20B)
6.c Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C1B(C2B,C3B,C4B,C5B,C6B), C15A(C16A,C17A,C18A,C19A,
 C20A), C15B(C16B,C17B,C18B,C19B,C20B)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C8B(H8BA,H8BB,H8BC)
;
_shelx_res_checksum              47036
_olex2_submission_special_instructions 'No special instructions were received'