#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/82/7128242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7128242
loop_
_publ_author_name
'Parvin, Nasrina'
'Sen, Nilanjana'
'Muhasina, Puthan Veetil'
'Tothadi, Srinu'
'Parameswaran, Pattiyil'
'Khan, Shabana'
_publ_section_title
;
 The diverse reactivity of NOBF₄ towards silylene, disilene,
 germylene and stannylene.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5008
_journal_page_last               5011
_journal_paper_doi               10.1039/d1cc01034d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C32 H66 F2 N2 Si6'
_chemical_formula_sum            'C32 H66 F2 N2 Si6'
_chemical_formula_weight         685.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-11 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                95.79(3)
_cell_angle_beta                 106.56(3)
_cell_angle_gamma                116.50(2)
_cell_formula_units_Z            1
_cell_length_a                   9.356(12)
_cell_length_b                   9.434(12)
_cell_length_c                   13.182(17)
_cell_measurement_reflns_used    1413
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.50
_cell_volume                     962(2)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2677
_diffrn_reflns_av_unetI/netI     0.3245
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11819
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.502
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1338 before and 0.0417 after correction. The Ratio of minimum to maximum transmission is 0.7164. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.2559
_refine_ls_R_factor_gt           0.1075
_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/[σ²(Fo²)+(0.0631P)²+1.4607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1402
_reflns_number_total             3369
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01034d2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7128241--7128247.cif.'
_cod_database_code               7128242
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C),
 C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C9(H9A,H9B,H9C),
  C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.5694(3) 0.5645(3) 0.6001(2) 0.0273(7) Uani 1 1 d . . . . .
Si2 Si 0.3319(3) 0.3099(3) 0.6987(2) 0.0287(7) Uani 1 1 d . . . . .
Si3 Si 0.7124(3) 0.4480(3) 0.7904(2) 0.0326(7) Uani 1 1 d . . . . .
F1 F 0.7729(5) 0.6275(5) 0.6202(4) 0.0398(13) Uani 1 1 d . . . . .
N1 N 0.5319(7) 0.4427(7) 0.6901(5) 0.0212(16) Uani 1 1 d . . . . .
C6 C 0.6018(11) 0.8622(10) 0.5513(7) 0.037(2) Uani 1 1 d . . . . .
H6A H 0.607085 0.967549 0.572288 0.055 Uiso 1 1 calc GR . . . .
H6B H 0.508845 0.797235 0.479797 0.055 Uiso 1 1 calc GR . . . .
H6C H 0.711457 0.881883 0.546458 0.055 Uiso 1 1 calc GR . . . .
C1 C 0.5670(11) 0.7669(10) 0.6389(7) 0.027(2) Uani 1 1 d . . . . .
C5 C 0.4010(10) 0.7309(10) 0.6536(7) 0.029(2) Uani 1 1 d . . . . .
C2 C 0.7011(10) 0.8628(9) 0.7528(7) 0.027(2) Uani 1 1 d . . . . .
C12 C 0.1418(10) 0.2922(11) 0.5889(7) 0.042(3) Uani 1 1 d . . . . .
H12A H 0.144322 0.397732 0.599362 0.064 Uiso 1 1 calc GR . . . .
H12B H 0.035720 0.207299 0.593188 0.064 Uiso 1 1 calc GR . . . .
H12C H 0.145712 0.262214 0.516818 0.064 Uiso 1 1 calc GR . . . .
C4 C 0.4359(12) 0.7777(10) 0.7619(8) 0.033(2) Uani 1 1 d . . . . .
C3 C 0.6199(12) 0.8612(10) 0.8239(7) 0.036(2) Uani 1 1 d . . . . .
C10 C 0.2379(10) 0.6755(11) 0.5599(7) 0.045(3) Uani 1 1 d . . . . .
H10A H 0.141976 0.636284 0.585699 0.068 Uiso 1 1 calc GR . . . .
H10B H 0.218845 0.586150 0.503455 0.068 Uiso 1 1 calc GR . . . .
H10C H 0.245369 0.767564 0.528902 0.068 Uiso 1 1 calc GR . . . .
C7 C 0.8885(11) 0.9638(11) 0.7721(8) 0.051(3) Uani 1 1 d . . . . .
H7A H 0.906980 1.056323 0.739509 0.077 Uiso 1 1 calc GR . . . .
H7B H 0.925180 0.895410 0.738252 0.077 Uiso 1 1 calc GR . . . .
H7C H 0.955624 1.005529 0.851248 0.077 Uiso 1 1 calc GR . . . .
C13 C 0.3190(10) 0.3871(10) 0.8300(7) 0.038(2) Uani 1 1 d . . . . .
H13A H 0.413629 0.500154 0.865577 0.057 Uiso 1 1 calc GR . . . .
H13B H 0.327731 0.317084 0.878797 0.057 Uiso 1 1 calc GR . . . .
H13C H 0.209003 0.384705 0.814678 0.057 Uiso 1 1 calc GR . . . .
C11 C 0.2928(11) 0.0938(10) 0.6829(7) 0.044(3) Uani 1 1 d . . . . .
H11A H 0.216534 0.028267 0.607342 0.066 Uiso 1 1 calc GR . . . .
H11B H 0.239059 0.045205 0.733714 0.066 Uiso 1 1 calc GR . . . .
H11C H 0.402604 0.095396 0.699412 0.066 Uiso 1 1 calc GR . . . .
C16 C 0.8851(13) 0.6526(11) 0.8780(9) 0.075(4) Uani 1 1 d . . . . .
H16A H 0.943716 0.716356 0.833749 0.112 Uiso 1 1 calc GR . . . .
H16B H 0.967775 0.641323 0.936862 0.112 Uiso 1 1 calc GR . . . .
H16C H 0.835996 0.709377 0.909969 0.112 Uiso 1 1 calc GR . . . .
C9 C 0.3068(12) 0.7667(11) 0.8151(8) 0.051(3) Uani 1 1 d . . . . .
H9A H 0.190262 0.707089 0.759151 0.077 Uiso 1 1 calc GR . . . .
H9B H 0.333616 0.877636 0.848191 0.077 Uiso 1 1 calc GR . . . .
H9C H 0.314046 0.708213 0.872107 0.077 Uiso 1 1 calc GR . . . .
C8 C 0.7010(13) 0.9358(11) 0.9452(7) 0.057(3) Uani 1 1 d . . . . .
H8A H 0.826469 0.993041 0.967762 0.086 Uiso 1 1 calc GR . . . .
H8B H 0.664946 0.849121 0.982823 0.086 Uiso 1 1 calc GR . . . .
H8C H 0.664853 1.014183 0.964423 0.086 Uiso 1 1 calc GR . . . .
C15 C 0.8079(12) 0.3454(12) 0.7312(7) 0.058(3) Uani 1 1 d . . . . .
H15A H 0.718304 0.233321 0.688049 0.087 Uiso 1 1 calc GR . . . .
H15B H 0.896382 0.341479 0.790408 0.087 Uiso 1 1 calc GR . . . .
H15C H 0.859953 0.406576 0.683659 0.087 Uiso 1 1 calc GR . . . .
C14 C 0.6511(14) 0.3379(15) 0.8953(9) 0.088(4) Uani 1 1 d . . . . .
H14A H 0.627693 0.402682 0.944349 0.132 Uiso 1 1 calc GR . . . .
H14B H 0.745703 0.323390 0.938202 0.132 Uiso 1 1 calc GR . . . .
H14C H 0.547866 0.230079 0.858007 0.132 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Si1 Si1 101.2(2) . 2_666 ?
F1 Si1 N1 102.6(3) . . ?
F1 Si1 C1 103.5(3) . . ?
N1 Si1 Si1 119.6(3) . 2_666 ?
N1 Si1 C1 114.7(3) . . ?
C1 Si1 Si1 112.1(3) . 2_666 ?
N1 Si2 C12 113.9(3) . . ?
N1 Si2 C13 111.0(3) . . ?
N1 Si2 C11 111.2(3) . . ?
C12 Si2 C11 105.0(4) . . ?
C13 Si2 C12 104.6(4) . . ?
C13 Si2 C11 110.8(4) . . ?
N1 Si3 C16 115.7(4) . . ?
N1 Si3 C15 113.4(4) . . ?
N1 Si3 C14 112.4(4) . . ?
C16 Si3 C14 101.5(5) . . ?
C15 Si3 C16 108.5(5) . . ?
C15 Si3 C14 104.2(5) . . ?
Si1 N1 Si2 127.8(4) . . ?
Si1 N1 Si3 118.8(4) . . ?
Si2 N1 Si3 113.5(3) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
C6 C1 Si1 108.9(5) . . ?
C5 C1 Si1 110.3(5) . . ?
C5 C1 C6 113.9(7) . . ?
C5 C1 C2 103.1(7) . . ?
C2 C1 Si1 107.8(5) . . ?
C2 C1 C6 112.6(7) . . ?
C4 C5 C1 108.0(7) . . ?
C4 C5 C10 128.5(8) . . ?
C10 C5 C1 122.9(8) . . ?
C3 C2 C1 108.8(7) . . ?
C3 C2 C7 128.6(8) . . ?
C7 C2 C1 121.7(8) . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C4 C3 110.8(8) . . ?
C5 C4 C9 126.3(9) . . ?
C3 C4 C9 122.5(8) . . ?
C2 C3 C4 108.6(8) . . ?
C2 C3 C8 127.4(9) . . ?
C4 C3 C8 124.0(9) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C16 H16A 109.5 . . ?
Si3 C16 H16B 109.5 . . ?
Si3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 Si1 2.475(6) 2_666 ?
Si1 F1 1.649(5) . ?
Si1 N1 1.732(7) . ?
Si1 C1 1.938(8) . ?
Si2 N1 1.773(7) . ?
Si2 C12 1.871(8) . ?
Si2 C13 1.867(8) . ?
Si2 C11 1.881(9) . ?
Si3 N1 1.800(7) . ?
Si3 C16 1.837(9) . ?
Si3 C15 1.833(9) . ?
Si3 C14 1.879(11) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 C1 1.552(11) . ?
C1 C5 1.510(11) . ?
C1 C2 1.512(11) . ?
C5 C4 1.349(11) . ?
C5 C10 1.487(11) . ?
C2 C3 1.362(11) . ?
C2 C7 1.500(11) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C4 C3 1.453(12) . ?
C4 C9 1.531(11) . ?
C3 C8 1.494(11) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168352719
