#------------------------------------------------------------------------------
#$Date: 2020-08-06 16:01:21 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254900 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/67/7126751.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_7126751
loop_
_publ_author_name
'Usui, Ryosuke'
'Sunada, Yusuke'
_publ_section_title
;
 Insertion of Ni(0) and Pd(0) precursors into the Si-Si bond of a disilane
 with two hypercoordinate silicon atoms.
;
_journal_issue                   60
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8464
_journal_page_last               8467
_journal_paper_doi               10.1039/d0cc03211e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C34 H34 N4 Si2'
_chemical_formula_sum            'C34 H34 N4 Si2'
_chemical_formula_weight         554.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-03-17 deposited with the CCDC.	2020-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.172(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   10.379(3)
_cell_length_b                   9.789(2)
_cell_length_c                   14.974(4)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    203
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     1468.3(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_diffrn_ambient_temperature      203
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11741
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         3.014
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0592P)²+1.0479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2732
_reflns_number_total             3277
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d0cc03211e2.cif
_cod_data_source_block           Ph2Si(m-Pz)2SiPh2
_cod_depositor_comments
'Adding full bibliography for 7126751--7126754.cif.'
_cod_original_cell_volume        1468.3(6)
_cod_database_code               7126751
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+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 0.39382(5) 0.04435(5) -0.02634(4) 0.02137(16) Uani 1 1 d . . . . .
N1 N 0.38438(15) -0.05300(16) 0.08737(11) 0.0225(3) Uani 1 1 d . . . . .
N2 N 0.50633(15) -0.11808(16) 0.11655(11) 0.0228(3) Uani 1 1 d . . . . .
C1 C 0.3046(2) -0.0992(2) 0.13864(14) 0.0275(4) Uani 1 1 d . . . . .
C2 C 0.3745(2) -0.1952(2) 0.20081(14) 0.0316(5) Uani 1 1 d . . . . .
H2 H 0.343265 -0.243942 0.245071 0.038 Uiso 1 1 calc R U . . .
C3 C 0.4999(2) -0.2049(2) 0.18442(13) 0.0277(4) Uani 1 1 d . . . . .
C4 C 0.1645(2) -0.0493(3) 0.12352(17) 0.0404(6) Uani 1 1 d . . . . .
H4A H 0.123267 -0.094107 0.166812 0.048 Uiso 1 1 calc R U . . .
H4B H 0.165046 0.048677 0.133205 0.048 Uiso 1 1 calc R U . . .
H4C H 0.114262 -0.070151 0.060735 0.048 Uiso 1 1 calc R U . . .
C5 C 0.6142(2) -0.2953(2) 0.23095(16) 0.0394(5) Uani 1 1 d . . . . .
H5A H 0.589234 -0.349908 0.277819 0.047 Uiso 1 1 calc R U . . .
H5B H 0.636329 -0.354966 0.185434 0.047 Uiso 1 1 calc R U . . .
H5C H 0.691054 -0.239436 0.259750 0.047 Uiso 1 1 calc R U . . .
C6 C 0.33063(19) 0.21561(19) 0.00102(13) 0.0231(4) Uani 1 1 d . . . . .
C7 C 0.4183(2) 0.3200(2) 0.04038(16) 0.0363(5) Uani 1 1 d . . . . .
H7 H 0.510635 0.305392 0.051597 0.044 Uiso 1 1 calc R U . . .
C8 C 0.3730(3) 0.4450(2) 0.06347(19) 0.0447(6) Uani 1 1 d . . . . .
H8 H 0.434478 0.513615 0.089959 0.054 Uiso 1 1 calc R U . . .
C9 C 0.2382(3) 0.4687(2) 0.04769(18) 0.0442(6) Uani 1 1 d . . . . .
H9 H 0.207357 0.552978 0.063898 0.053 Uiso 1 1 calc R U . . .
C10 C 0.1490(2) 0.3681(2) 0.00804(18) 0.0418(6) Uani 1 1 d . . . . .
H10 H 0.056823 0.384073 -0.003472 0.050 Uiso 1 1 calc R U . . .
C11 C 0.1946(2) 0.2430(2) -0.01508(15) 0.0329(5) Uani 1 1 d . . . . .
H11 H 0.132447 0.175276 -0.042179 0.039 Uiso 1 1 calc R U . . .
C12 C 0.25779(19) -0.05458(19) -0.10988(13) 0.0237(4) Uani 1 1 d . . . . .
C13 C 0.1931(2) -0.0033(2) -0.19669(15) 0.0331(5) Uani 1 1 d . . . . .
H13 H 0.220411 0.081096 -0.215415 0.040 Uiso 1 1 calc R U . . .
C14 C 0.0893(2) -0.0735(3) -0.25646(16) 0.0397(6) Uani 1 1 d . . . . .
H14 H 0.046592 -0.035565 -0.314303 0.048 Uiso 1 1 calc R U . . .
C15 C 0.0487(2) -0.1980(3) -0.23148(17) 0.0418(6) Uani 1 1 d . . . . .
H15 H -0.023176 -0.244357 -0.271157 0.050 Uiso 1 1 calc R U . . .
C16 C 0.1146(3) -0.2542(3) -0.14750(18) 0.0474(6) Uani 1 1 d . . . . .
H16 H 0.090179 -0.341257 -0.131118 0.057 Uiso 1 1 calc R U . . .
C17 C 0.2166(2) -0.1831(2) -0.08706(15) 0.0351(5) Uani 1 1 d . . . . .
H17 H 0.258993 -0.222126 -0.029503 0.042 Uiso 1 1 calc R U . . .
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.0817 0.0704
;
International Tables for Crystallography
(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
C6 Si1 C12 110.95(8) . . ?
C6 Si1 N1 98.23(8) . . ?
C12 Si1 N1 97.26(8) . . ?
C6 Si1 N2 95.47(8) . 3_655 ?
C12 Si1 N2 99.44(8) . 3_655 ?
N1 Si1 N2 152.95(7) . 3_655 ?
C6 Si1 Si1 128.05(7) . 3_655 ?
C12 Si1 Si1 120.98(7) . 3_655 ?
N1 Si1 Si1 77.43(5) . 3_655 ?
N2 Si1 Si1 75.75(5) 3_655 3_655 ?
C1 N1 N2 108.29(15) . . ?
C1 N1 Si1 146.12(14) . . ?
N2 N1 Si1 104.30(11) . . ?
C3 N2 N1 108.00(15) . . ?
C3 N2 Si1 149.59(14) . 3_655 ?
N1 N2 Si1 102.11(11) . 3_655 ?
N1 C1 C2 108.63(18) . . ?
N1 C1 C4 121.55(19) . . ?
C2 C1 C4 129.82(19) . . ?
C1 C2 C3 106.07(18) . . ?
C1 C2 H2 127.0 . . ?
C3 C2 H2 127.0 . . ?
N2 C3 C2 109.00(18) . . ?
N2 C3 C5 122.48(19) . . ?
C2 C3 C5 128.52(19) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 116.85(18) . . ?
C7 C6 Si1 121.28(15) . . ?
C11 C6 Si1 121.85(15) . . ?
C8 C7 C6 121.8(2) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C9 C8 C7 120.1(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 120.3(2) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C6 121.5(2) . . ?
C10 C11 H11 119.3 . . ?
C6 C11 H11 119.3 . . ?
C13 C12 C17 116.66(18) . . ?
C13 C12 Si1 121.87(15) . . ?
C17 C12 Si1 121.47(15) . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C15 C14 C13 120.3(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.2(2) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C15 C16 C17 120.5(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C12 121.4(2) . . ?
C16 C17 H17 119.3 . . ?
C12 C17 H17 119.3 . . ?
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 C6 1.884(2) . ?
Si1 C12 1.8899(19) . ?
Si1 N1 1.9759(17) . ?
Si1 N2 2.0377(17) 3_655 ?
Si1 Si1 2.3073(11) 3_655 ?
N1 C1 1.346(2) . ?
N1 N2 1.382(2) . ?
N2 C3 1.340(2) . ?
C1 C2 1.387(3) . ?
C1 C4 1.494(3) . ?
C2 C3 1.390(3) . ?
C2 H2 0.9400 . ?
C3 C5 1.497(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 C7 1.392(3) . ?
C6 C11 1.394(3) . ?
C7 C8 1.386(3) . ?
C7 H7 0.9400 . ?
C8 C9 1.376(4) . ?
C8 H8 0.9400 . ?
C9 C10 1.375(4) . ?
C9 H9 0.9400 . ?
C10 C11 1.389(3) . ?
C10 H10 0.9400 . ?
C11 H11 0.9400 . ?
C12 C13 1.391(3) . ?
C12 C17 1.400(3) . ?
C13 C14 1.389(3) . ?
C13 H13 0.9400 . ?
C14 C15 1.373(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.379(4) . ?
C15 H15 0.9400 . ?
C16 C17 1.386(3) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 C3 0.9(2) . . . . ?
Si1 N1 N2 C3 -169.71(13) . . . . ?
C1 N1 N2 Si1 176.52(12) . . . 3_655 ?
Si1 N1 N2 Si1 5.94(11) . . . 3_655 ?
N2 N1 C1 C2 -0.4(2) . . . . ?
Si1 N1 C1 C2 163.03(19) . . . . ?
N2 N1 C1 C4 -179.47(18) . . . . ?
Si1 N1 C1 C4 -16.0(4) . . . . ?
N1 C1 C2 C3 -0.1(2) . . . . ?
C4 C1 C2 C3 178.8(2) . . . . ?
N1 N2 C3 C2 -1.0(2) . . . . ?
Si1 N2 C3 C2 -172.5(2) 3_655 . . . ?
N1 N2 C3 C5 178.59(18) . . . . ?
Si1 N2 C3 C5 7.0(4) 3_655 . . . ?
C1 C2 C3 N2 0.7(2) . . . . ?
C1 C2 C3 C5 -178.8(2) . . . . ?
C12 Si1 C6 C7 -162.87(17) . . . . ?
N1 Si1 C6 C7 96.05(18) . . . . ?
N2 Si1 C6 C7 -60.57(18) 3_655 . . . ?
Si1 Si1 C6 C7 15.6(2) 3_655 . . . ?
C12 Si1 C6 C11 18.61(19) . . . . ?
N1 Si1 C6 C11 -82.47(17) . . . . ?
N2 Si1 C6 C11 120.92(17) 3_655 . . . ?
Si1 Si1 C6 C11 -162.91(14) 3_655 . . . ?
C11 C6 C7 C8 0.6(3) . . . . ?
Si1 C6 C7 C8 -177.94(19) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C7 C8 C9 C10 -0.7(4) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C10 C11 C6 0.0(4) . . . . ?
C7 C6 C11 C10 -0.7(3) . . . . ?
Si1 C6 C11 C10 177.91(17) . . . . ?
C6 Si1 C12 C13 58.29(19) . . . . ?
N1 Si1 C12 C13 160.02(17) . . . . ?
N2 Si1 C12 C13 -41.34(18) 3_655 . . . ?
Si1 Si1 C12 C13 -120.32(16) 3_655 . . . ?
C6 Si1 C12 C17 -121.33(17) . . . . ?
N1 Si1 C12 C17 -19.60(18) . . . . ?
N2 Si1 C12 C17 139.04(17) 3_655 . . . ?
Si1 Si1 C12 C17 60.07(19) 3_655 . . . ?
C17 C12 C13 C14 2.4(3) . . . . ?
Si1 C12 C13 C14 -177.20(17) . . . . ?
C12 C13 C14 C15 -1.0(4) . . . . ?
C13 C14 C15 C16 -1.8(4) . . . . ?
C14 C15 C16 C17 3.0(4) . . . . ?
C15 C16 C17 C12 -1.5(4) . . . . ?
C13 C12 C17 C16 -1.2(3) . . . . ?
Si1 C12 C17 C16 178.42(19) . . . . ?
