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_7225393
_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(C22 H17 B O2 Si)'
_chemical_formula_sum            'C44 H34 B2 O4 Si2'
_chemical_formula_weight         704.51
_chemical_name_systematic
'4,8-di(naphthalen-2-yl)-2,2,6,6-tetraphenyl-1,3,5,7,2,6,4,8-tetraoxadisiladiborocane 4,8-di(naphthalen-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             2014-12-19
_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                82.604(9)
_cell_angle_beta                 87.095(7)
_cell_angle_gamma                83.427(9)
_cell_formula_units_Z            2
_cell_length_a                   9.269(6)
_cell_length_b                   10.361(7)
_cell_length_c                   19.149(12)
_cell_measurement_reflns_used    1066
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      25.579
_cell_measurement_theta_min      2.424
_cell_volume                     1811(2)
_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      150.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21130
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         1.994
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.8971.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         8155
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+2.2011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6039
_reflns_number_total             8155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra02080a2.cif
_cod_data_source_block           gp53
_cod_original_cell_volume        1810.6(19)
_cod_database_code               7225393
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.945
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Si1A-C11A \\sim Si1A-C11B
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma of 0.1
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B
\\sim C7B \\sim C8B \\sim C9B \\sim C10B: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C11B \\sim
C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C1B, C2B, C3B, C4B, C5B,
 C6B, C7B, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C11A, C12A, C13A, C14A, C15A, C16A, C11B, C12B, C13B, C14B, C15B, C16B
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Same fragment restrains
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A}
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B}
7. Others
 Sof(C11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=
 Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=
 Sof(C4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=
 Sof(H8B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10B)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=
 Sof(H10A)=Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C1A(H1A), C2A(H2A), C5A(H5A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A),
 C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C12B(H12B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C18A(H18A), C19A(H19A),
 C20A(H20A), C21A(H21A), C22A(H22A), C2B(H2B), C5B(H5B), C6B(H6B), C7B(H7B),
 C8B(H8B), C9B(H9B), C10B(H10B)
8.b Fitted hexagon refined as free rotating group:
 C11A(C12A,C13A,C14A,C15A,C16A), C11B(C12B,C13B,C14B,C15B,C16B)
;
_shelx_res_checksum              15396
_olex2_submission_special_instructions 'No special instructions were received'