#------------------------------------------------------------------------------
#$Date: 2019-11-26 12:06:04 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243338 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/35/4133583.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_4133583
loop_
_publ_author_name
'Kostenko, Arseni'
'Driess, Matthias'
_publ_section_title
;
 Geometrically Compelled Disilene with λ⁴-Coordinate
 SiII Atoms.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16962
_journal_page_last               16966
_journal_paper_doi               10.1021/jacs.8b11393
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C42 H54 N4 Si2'
_chemical_formula_sum            'C42 H54 N4 Si2'
_chemical_formula_weight         671.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5089(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.12662(14)
_cell_length_b                   10.49281(11)
_cell_length_c                   25.5869(3)
_cell_measurement_reflns_used    8319
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.4590
_cell_measurement_theta_min      3.4520
_cell_volume                     3780.96(7)
_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    'ShelXD-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13011
_diffrn_reflns_theta_full        73.59
_diffrn_reflns_theta_max         73.59
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0537P)²+2.6349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                3539
_reflns_number_total             3756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b11393_si_002.cif
_cod_data_source_block           cu-2517
_cod_database_code               4133583
_oxdiff_exptl_absorpt_empirical_full_min 0.807
_oxdiff_exptl_absorpt_empirical_full_max 1.616
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,
 H3AB,H3AC), C4AA(H4AA,H4AB,H4AC), C5AA(H5AA,H5AB,H5AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'
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_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Si1 Si 0.52014(2) 0.11225(3) 0.800921(13) 0.02229(11) Uani 1 d 1 . . .
N2 N 0.41454(7) 0.17117(10) 0.83426(4) 0.0234(2) Uani 1 d 1 . . .
N3 N 0.55217(8) 0.13874(10) 0.87427(4) 0.0251(2) Uani 1 d 1 . . .
C0AA C 0.66568(12) 0.31398(15) 0.89569(8) 0.0475(4) Uani 1 d 1 . . .
H0AA H 0.6638 0.3347 0.8591 0.071 Uiso 1 calc 1 GR . .
H0AB H 0.7276 0.3327 0.9121 0.071 Uiso 1 calc 1 GR . .
H0AC H 0.6190 0.3635 0.9120 0.071 Uiso 1 calc 1 GR . .
C1 C 0.5000 -0.13163(16) 0.7500 0.0215(3) Uani 1 d 2 S T P
C1AA C 0.64926(13) 0.13769(19) 0.95984(6) 0.0476(4) Uani 1 d 1 . . .
H1AA H 0.6074 0.1920 0.9775 0.071 Uiso 1 calc 1 GR . .
H1AB H 0.7131 0.1485 0.9750 0.071 Uiso 1 calc 1 GR . .
H1AC H 0.6303 0.0505 0.9635 0.071 Uiso 1 calc 1 GR . .
C2AA C 0.71855(11) 0.09491(18) 0.87572(7) 0.0456(4) Uani 1 d 1 . . .
H2AA H 0.7061 0.0057 0.8800 0.068 Uiso 1 calc 1 GR . .
H2AB H 0.7806 0.1148 0.8916 0.068 Uiso 1 calc 1 GR . .
H2AC H 0.7156 0.1151 0.8390 0.068 Uiso 1 calc 1 GR . .
C3AA C 0.28662(10) 0.29431(15) 0.78866(7) 0.0408(4) Uani 1 d 1 . . .
H3AA H 0.3019 0.3690 0.8093 0.061 Uiso 1 calc 1 GR . .
H3AB H 0.2202 0.2946 0.7775 0.061 Uiso 1 calc 1 GR . .
H3AC H 0.3230 0.2941 0.7585 0.061 Uiso 1 calc 1 GR . .
C4 C 0.49545(9) -0.34025(12) 0.79537(5) 0.0264(3) Uani 1 d 1 . . .
C4AA C 0.28121(10) 0.05723(14) 0.78984(6) 0.0333(3) Uani 1 d 1 . . .
H4AA H 0.3159 0.0537 0.7591 0.050 Uiso 1 calc 1 GR . .
H4AB H 0.2144 0.0602 0.7797 0.050 Uiso 1 calc 1 GR . .
H4AC H 0.2952 -0.0171 0.8109 0.050 Uiso 1 calc 1 GR . .
C5 C 0.50003(9) -0.06799(12) 0.79948(5) 0.0239(3) Uani 1 d 1 . . .
C5AA C 0.25403(10) 0.17609(17) 0.87021(6) 0.0417(4) Uani 1 d 1 . . .
H5AA H 0.2722 0.1036 0.8916 0.063 Uiso 1 calc 1 GR . .
H5AB H 0.1873 0.1718 0.8598 0.063 Uiso 1 calc 1 GR . .
H5AC H 0.2675 0.2528 0.8898 0.063 Uiso 1 calc 1 GR . .
C6 C 0.42408(10) 0.38632(13) 0.92680(5) 0.0295(3) Uani 1 d 1 . . .
H6 H 0.4348 0.4332 0.8970 0.035 Uiso 1 calc 1 R . .
C7 C 0.5000 -0.26534(16) 0.7500 0.0225(3) Uani 1 d 2 S T P
C8 C 0.46614(9) 0.18836(11) 0.87980(5) 0.0239(3) Uani 1 d 1 . . .
C9 C 0.43628(9) 0.25526(13) 0.92706(5) 0.0264(3) Uani 1 d 1 . . .
C10 C 0.64450(9) 0.17282(13) 0.90197(5) 0.0281(3) Uani 1 d 1 . . .
C11 C 0.31004(9) 0.17610(12) 0.82138(5) 0.0269(3) Uani 1 d 1 . . .
C12 C 0.49553(10) -0.14367(13) 0.84370(5) 0.0288(3) Uani 1 d 1 . . .
H12 H 0.4950 -0.1034 0.8761 0.035 Uiso 1 calc 1 R . .
C13 C 0.37806(12) 0.37775(16) 1.01509(6) 0.0414(4) Uani 1 d 1 . . .
H13 H 0.3581 0.4189 1.0445 0.050 Uiso 1 calc 1 R . .
C14 C 0.49165(10) -0.27902(13) 0.84256(5) 0.0315(3) Uani 1 d 1 . . .
H14 H 0.4866 -0.3253 0.8732 0.038 Uiso 1 calc 1 R . .
C15 C 0.39588(10) 0.44761(15) 0.97114(6) 0.0368(3) Uani 1 d 1 . . .
H15 H 0.3890 0.5358 0.9712 0.044 Uiso 1 calc 1 R . .
C16 C 0.49703(10) -0.47946(12) 0.78004(6) 0.0339(3) Uani 1 d 1 . . .
H16A H 0.4398 -0.5222 0.7893 0.041 Uiso 1 calc 1 R . .
H16B H 0.5517 -0.5221 0.7975 0.041 Uiso 1 calc 1 R . .
C19 C 0.41960(11) 0.18604(15) 0.97192(6) 0.0360(3) Uani 1 d 1 . . .
H19 H 0.4286 0.0982 0.9725 0.043 Uiso 1 calc 1 R . .
C20 C 0.38969(12) 0.24774(17) 1.01560(6) 0.0425(4) Uani 1 d 1 . . .
H20 H 0.3775 0.2011 1.0453 0.051 Uiso 1 calc 1 R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
N2 Si1 Si1 109.44(4) . 2_656
N2 Si1 N3 69.06(5) . .
N2 Si1 C5 102.24(5) . .
N2 Si1 C8 34.61(4) . .
N3 Si1 Si1 171.56(3) . 2_656
N3 Si1 C8 34.71(5) . .
C5 Si1 Si1 87.74(4) . 2_656
C5 Si1 N3 100.70(5) . .
C5 Si1 C8 107.13(5) . .
C8 Si1 Si1 142.43(4) . 2_656
C8 N2 Si1 92.41(8) . .
C8 N2 C11 130.66(11) . .
C11 N2 Si1 136.03(8) . .
C8 N3 Si1 90.77(8) . .
C8 N3 C10 128.95(11) . .
C10 N3 Si1 129.51(9) . .
C5 C1 C5 124.38(16) 2_656 .
C7 C1 C5 117.81(8) . .
C7 C1 C5 117.81(8) . 2_656
C7 C4 C16 108.83(12) . .
C14 C4 C7 118.14(12) . .
C14 C4 C16 133.03(12) . .
C1 C5 Si1 117.91(10) . .
C12 C5 Si1 124.49(10) . .
C12 C5 C1 117.22(12) . .
C9 C6 C15 119.93(13) . .
C1 C7 C4 123.95(8) . .
C1 C7 C4 123.95(8) . 2_656
C4 C7 C4 112.10(16) . 2_656
N2 C8 Si1 52.98(6) . .
N2 C8 N3 107.00(11) . .
N2 C8 C9 127.01(11) . .
N3 C8 Si1 54.52(6) . .
N3 C8 C9 125.93(11) . .
C9 C8 Si1 171.59(9) . .
C6 C9 C8 120.50(12) . .
C6 C9 C19 119.47(12) . .
C19 C9 C8 120.03(12) . .
N3 C10 C0AA 110.98(11) . .
N3 C10 C1AA 112.18(12) . .
N3 C10 C2AA 105.61(11) . .
C0AA C10 C1AA 110.14(14) . .
C0AA C10 C2AA 109.15(14) . .
C1AA C10 C2AA 108.62(13) . .
N2 C11 C3AA 108.66(10) . .
N2 C11 C4AA 107.94(10) . .
N2 C11 C5AA 112.76(11) . .
C3AA C11 C4AA 109.82(12) . .
C3AA C11 C5AA 110.23(12) . .
C4AA C11 C5AA 107.37(11) . .
C5 C12 C14 123.98(12) . .
C20 C13 C15 120.34(14) . .
C4 C14 C12 118.80(12) . .
C13 C15 C6 120.08(14) . .
C4 C16 C16 105.12(8) . 2_656
C20 C19 C9 120.17(14) . .
C13 C20 C19 120.00(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Si1 2.6231(7) 2_656
Si1 N2 1.8802(11) .
Si1 N3 1.9159(11) .
Si1 C5 1.9124(13) .
Si1 C8 2.3527(13) .
N2 C8 1.3374(16) .
N2 C11 1.4879(16) .
N3 C8 1.3398(17) .
N3 C10 1.4786(16) .
C0AA C10 1.522(2) .
C1 C5 1.4313(14) .
C1 C5 1.4312(14) 2_656
C1 C7 1.403(2) .
C1AA C10 1.522(2) .
C2AA C10 1.524(2) .
C3AA C11 1.518(2) .
C4 C7 1.4076(16) .
C4 C14 1.372(2) .
C4 C16 1.5130(18) .
C4AA C11 1.5235(18) .
C5 C12 1.3880(18) .
C5AA C11 1.5305(19) .
C6 C9 1.3859(19) .
C6 C15 1.3894(19) .
C7 C4 1.4077(16) 2_656
C8 C9 1.4876(17) .
C9 C19 1.3940(19) .
C12 C14 1.4215(19) .
C13 C15 1.382(2) .
C13 C20 1.374(2) .
C16 C16 1.546(3) 2_656
C19 C20 1.386(2) .
