#------------------------------------------------------------------------------
#$Date: 2019-11-26 12:05:20 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243336 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/35/4133581.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_4133581
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 O2 Si2'
_chemical_formula_sum            'C42 H54 N4 O2 Si2'
_chemical_formula_weight         703.07
_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     iterative
_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                 98.675(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7680(5)
_cell_length_b                   10.4696(4)
_cell_length_c                   25.1558(8)
_cell_measurement_reflns_used    2503
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.4520
_cell_measurement_theta_min      3.5240
_cell_volume                     3845.0(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  multi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12974
_diffrn_reflns_theta_full        73.63
_diffrn_reflns_theta_max         73.63
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0544P)²+1.7067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                2697
_reflns_number_total             3838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b11393_si_006.cif
_cod_data_source_block           cu-2947
_cod_database_code               4133581
_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:
 C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C16(H16), C18(H18)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_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 0.01748(4) 0.10036(5) 0.20418(2) 0.02046(15) Uani 1 d 1 . . .
O1 O 0.07608(10) 0.13162(16) 0.26638(6) 0.0284(4) Uani 1 d 1 . . .
N4 N 0.10827(12) 0.16066(18) 0.16566(7) 0.0224(4) Uani 1 d 1 . . .
N5 N -0.03379(12) 0.15595(18) 0.13417(7) 0.0244(4) Uani 1 d 1 . . .
C6 C 0.01688(15) -0.3520(2) 0.20577(9) 0.0247(5) Uani 1 d 1 . . .
C7 C 0.04774(15) 0.19077(19) 0.12273(8) 0.0209(4) Uani 1 d 1 . . .
C8 C 0.07705(15) 0.3858(2) 0.07264(9) 0.0270(5) Uani 1 d 1 . . .
H8 H 0.0663 0.4334 0.1023 0.032 Uiso 1 calc 1 R . .
C9 C 0.03523(16) -0.2912(2) 0.16060(9) 0.0292(5) Uani 1 d 1 . . .
H9 H 0.0470 -0.3377 0.1309 0.035 Uiso 1 calc 1 R . .
C10 C 0.03593(15) -0.1554(2) 0.15976(9) 0.0268(5) Uani 1 d 1 . . .
H10 H 0.0486 -0.1152 0.1288 0.032 Uiso 1 calc 1 R . .
C11 C 0.06908(15) 0.2543(2) 0.07336(9) 0.0232(5) Uani 1 d 1 . . .
C12 C 0.11650(18) 0.3770(3) -0.01621(10) 0.0438(7) Uani 1 d 1 . . .
H12 H 0.1327 0.4182 -0.0461 0.053 Uiso 1 calc 1 R . .
C13 C 0.08432(18) 0.1840(3) 0.02864(10) 0.0359(6) Uani 1 d 1 . . .
H13 H 0.0785 0.0956 0.0287 0.043 Uiso 1 calc 1 R . .
C14 C 0.20940(14) 0.1754(2) 0.17734(9) 0.0237(5) Uani 1 d 1 . . .
C15 C -0.12709(15) 0.1720(2) 0.10367(9) 0.0258(5) Uani 1 d 1 . . .
C16 C 0.1081(2) 0.2455(3) -0.01609(11) 0.0458(7) Uani 1 d 1 . . .
H16 H 0.1184 0.1983 -0.0459 0.055 Uiso 1 calc 1 R . .
C17 C 0.23090(16) 0.2984(2) 0.20918(11) 0.0351(6) Uani 1 d 1 . . .
H17A H 0.2112 0.3703 0.1868 0.053 Uiso 1 calc 1 GR . .
H17B H 0.2957 0.3040 0.2210 0.053 Uiso 1 calc 1 GR . .
H17C H 0.1994 0.2982 0.2399 0.053 Uiso 1 calc 1 GR . .
C18 C 0.10097(17) 0.4471(3) 0.02788(10) 0.0376(6) Uani 1 d 1 . . .
H18 H 0.1065 0.5356 0.0276 0.045 Uiso 1 calc 1 R . .
C19 C 0.01900(14) -0.07938(19) 0.20196(9) 0.0208(4) Uani 1 d 1 . . .
C20 C 0.00899(16) -0.4919(2) 0.22036(10) 0.0297(5) Uani 1 d 1 . . .
H20A H 0.0652 -0.5372 0.2171 0.036 Uiso 1 calc 1 R . .
H20B H -0.0413 -0.5322 0.1971 0.036 Uiso 1 calc 1 R . .
C21 C 0.25684(17) 0.1759(3) 0.12736(10) 0.0377(6) Uani 1 d 1 . . .
H21A H 0.2378 0.1025 0.1057 0.057 Uiso 1 calc 1 GR . .
H21B H 0.3220 0.1734 0.1381 0.057 Uiso 1 calc 1 GR . .
H21C H 0.2405 0.2521 0.1069 0.057 Uiso 1 calc 1 GR . .
C22 C 0.24504(16) 0.0606(2) 0.21161(10) 0.0332(6) Uani 1 d 1 . . .
H22A H 0.2176 0.0595 0.2439 0.050 Uiso 1 calc 1 GR . .
H22B H 0.3104 0.0666 0.2209 0.050 Uiso 1 calc 1 GR . .
H22C H 0.2296 -0.0166 0.1917 0.050 Uiso 1 calc 1 GR . .
C24 C -0.18554(19) 0.0649(3) 0.12202(12) 0.0480(8) Uani 1 d 1 . . .
H24A H -0.1621 -0.0162 0.1126 0.072 Uiso 1 calc 1 GR . .
H24B H -0.2477 0.0742 0.1047 0.072 Uiso 1 calc 1 GR . .
H24C H -0.1835 0.0693 0.1603 0.072 Uiso 1 calc 1 GR . .
C25 C -0.1643(2) 0.3004(3) 0.11787(14) 0.0565(9) Uani 1 d 1 . . .
H25A H -0.1604 0.3072 0.1562 0.085 Uiso 1 calc 1 GR . .
H25B H -0.2272 0.3079 0.1015 0.085 Uiso 1 calc 1 GR . .
H25C H -0.1291 0.3674 0.1049 0.085 Uiso 1 calc 1 GR . .
C26 C -0.1304(2) 0.1587(4) 0.04306(10) 0.0528(8) Uani 1 d 1 . . .
H26A H -0.0996 0.2299 0.0297 0.079 Uiso 1 calc 1 GR . .
H26B H -0.1931 0.1570 0.0260 0.079 Uiso 1 calc 1 GR . .
H26C H -0.1007 0.0808 0.0353 0.079 Uiso 1 calc 1 GR . .
C1 C 0.0000 -0.2780(3) 0.2500 0.0201(6) Uani 1 d 2 S T P
C2 C 0.0000 -0.1430(3) 0.2500 0.0191(6) Uani 1 d 2 S T P
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'
O O 0.0492 0.0322 '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
O1 Si1 Si1 44.26(5) 2 2
O1 Si1 Si1 44.05(5) . 2
O1 Si1 O1 84.04(9) 2 .
O1 Si1 N4 148.53(9) 2 .
O1 Si1 N4 96.10(8) . .
O1 Si1 N5 96.24(8) 2 .
O1 Si1 N5 150.40(9) . .
O1 Si1 C7 125.13(8) 2 .
O1 Si1 C7 125.77(8) . .
O1 Si1 C19 102.71(9) 2 .
O1 Si1 C19 102.29(9) . .
N4 Si1 Si1 139.26(7) . 2
N4 Si1 N5 68.56(8) . .
N4 Si1 C7 34.29(7) . .
N4 Si1 C19 107.94(9) . .
N5 Si1 Si1 139.90(7) . 2
N5 Si1 C7 34.28(7) . .
C7 Si1 Si1 156.35(5) . 2
C19 Si1 Si1 91.91(7) . 2
C19 Si1 N5 106.46(9) . .
C19 Si1 C7 111.74(9) . .
Si1 O1 Si1 91.69(8) 2 .
C7 N4 Si1 93.09(13) . .
C7 N4 C14 131.86(18) . .
C14 N4 Si1 135.02(14) . .
C7 N5 Si1 92.14(13) . .
C7 N5 C15 131.15(19) . .
C15 N5 Si1 136.37(15) . .
C9 C6 C20 133.1(2) . .
C9 C6 C1 118.8(2) . .
C1 C6 C20 108.1(2) . .
N4 C7 Si1 52.62(11) . .
N4 C7 C11 125.70(19) . .
N5 C7 Si1 53.58(11) . .
N5 C7 N4 106.16(18) . .
N5 C7 C11 128.11(19) . .
C11 C7 Si1 176.61(16) . .
C11 C8 C18 120.3(2) . .
C6 C9 C10 118.8(2) . .
C19 C10 C9 124.3(2) . .
C8 C11 C7 119.1(2) . .
C8 C11 C13 119.4(2) . .
C13 C11 C7 121.4(2) . .
C18 C12 C16 120.2(2) . .
C16 C13 C11 120.2(3) . .
N4 C14 C17 108.39(18) . .
N4 C14 C21 114.16(18) . .
N4 C14 C22 106.28(18) . .
C17 C14 C21 110.2(2) . .
C17 C14 C22 110.0(2) . .
C22 C14 C21 107.78(19) . .
N5 C15 C24 106.48(19) . .
N5 C15 C25 108.72(19) . .
N5 C15 C26 113.3(2) . .
C25 C15 C24 109.8(2) . .
C25 C15 C26 111.0(2) . .
C26 C15 C24 107.5(2) . .
C12 C16 C13 119.8(3) . .
C12 C18 C8 120.0(2) . .
C10 C19 Si1 127.14(17) . .
C10 C19 C2 117.3(2) . .
C2 C19 Si1 115.56(17) . .
C6 C20 C20 105.20(13) . 2
C6 C1 C6 113.3(3) . 2
C6 C1 C2 123.37(14) 2 .
C6 C1 C2 123.37(14) . .
C19 C2 C19 125.1(3) 2 .
C1 C2 C19 117.48(13) . 2
C1 C2 C19 117.47(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Si1 2.4370(11) 2
Si1 O1 1.6951(16) 2
Si1 O1 1.7017(16) .
Si1 N4 1.8782(18) .
Si1 N5 1.9005(19) .
Si1 C7 2.360(2) .
Si1 C19 1.883(2) .
O1 Si1 1.6950(16) 2
N4 C7 1.332(3) .
N4 C14 1.486(3) .
N5 C7 1.330(3) .
N5 C15 1.482(3) .
C6 C9 1.365(3) .
C6 C20 1.519(3) .
C6 C1 1.408(3) .
C7 C11 1.484(3) .
C8 C11 1.383(3) .
C8 C18 1.387(3) .
C9 C10 1.422(3) .
C10 C19 1.379(3) .
C11 C13 1.390(3) .
C12 C16 1.382(4) .
C12 C18 1.378(4) .
C13 C16 1.387(4) .
C14 C17 1.524(3) .
C14 C21 1.529(3) .
C14 C22 1.526(3) .
C15 C24 1.529(3) .
C15 C25 1.515(4) .
C15 C26 1.524(3) .
C19 C2 1.444(2) .
C20 C20 1.554(5) 2
C1 C6 1.408(3) 2
C1 C2 1.413(4) .
C2 C19 1.444(2) 2
