#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:24:23 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228842 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/00/1550065.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_1550065
loop_
_publ_author_name
'Le Roy, Jennifer J.'
'Cremers, Jonathan'
'Thomlinson, Isabel A.'
'Slota, Michael'
'Myers, William K.'
'Horton, Peter H.'
'Coles, Simon J.'
'Anderson, Harry L.'
'Bogani, Lapo'
_publ_section_title
;
 Tailored homo- and hetero- lanthanide porphyrin dimers: a synthetic
 strategy for integrating multiple spintronic functionalities into a
 single molecule.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              8474
_journal_page_last               8481
_journal_paper_doi               10.1039/c8sc03762k
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C72 H92 N6 Si2'
_chemical_formula_sum            'C72 H92 N6 Si2'
_chemical_formula_weight         1097.69
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.02.06 svn.r3384 for OlexSys, GUI svn.r5312)
;
_audit_update_record
;
2017-07-27 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                104.289(6)
_cell_angle_beta                 99.208(5)
_cell_angle_gamma                101.826(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4966(5)
_cell_length_b                   12.3975(8)
_cell_length_c                   13.2265(10)
_cell_measurement_reflns_used    6076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8160
_cell_measurement_theta_min      2.3070
_cell_volume                     1591.78(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  94.00   1.00   10.00    --    5.00  38.00 -60.00  109
  2  ω    -84.00  25.00   1.00   10.00    --    5.00 -38.00 -30.00  109
  3  ω    -31.00  83.00   1.00   10.00    --   -6.00  57.00-150.00  114
  4  ω    -95.00  23.00   1.00   10.00    --   -6.00 -72.00 -90.00  118
  5  ω    -95.00  23.00   1.00   10.00    --   -6.00 -72.00  90.00  118
  6  ω    -31.00  16.00   1.00   10.00    --   -6.00  57.00  90.00   47
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002165000
_diffrn_orient_matrix_UB_12      0.0557578000
_diffrn_orient_matrix_UB_13      0.0306807000
_diffrn_orient_matrix_UB_21      -0.0177308000
_diffrn_orient_matrix_UB_22      -0.0227879000
_diffrn_orient_matrix_UB_23      0.0414807000
_diffrn_orient_matrix_UB_31      0.0685509000
_diffrn_orient_matrix_UB_32      0.0100483000
_diffrn_orient_matrix_UB_33      0.0236492000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27097
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.306
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   'iridescent dark'
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5633
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0734
_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)+(0.1017P)²+1.4642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4022
_reflns_number_total             5633
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc03762k2.cif
_cod_data_source_block           P1star2H
_cod_depositor_comments
'Adding full bibliography for 1550065--1550077.cif.'
_cod_original_cell_volume        1591.78(18)
_cod_database_code               1550065
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C72 H92 N6 Si2'
_chemical_oxdiff_usercomment     Por-CN
_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.
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C33 \\sim Si1-C33B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33B) = Uanis(C34B) = Uanis(C35B) = Uanis(C36B)
4. Same fragment restrains
{N3, C33, C34, C35, C36} sigma for 1-2: 0.02, 1-3: 0.04
as
{N3B, C33B, C34B, C35B, C36B}
5. Others
 Sof(N3B)=Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=
 Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=1-FVAR(1)
 Sof(N3)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=FVAR(1)
 Fixed Sof: H1(0.5) H2(0.5)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C30(H30)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C33B(H33C,H33D), C34B(H34C,
 H34D), C35B(H35C,H35D)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C3(H3), C7(H7), C8(H8), C12(H12), C14(H14), C16(H16)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.581
_oxdiff_exptl_absorpt_empirical_full_min 0.568
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.28849(9) 0.76876(9) 0.59694(7) 0.0430(3) Uani 1 1 d D . . .
N1 N 1.0909(2) 0.9657(2) 0.36975(18) 0.0259(6) Uani 1 1 d . . . .
H1 H 1.0477 0.9852 0.4203 0.031 Uiso 0.5 1 calc R P . .
N2 N 0.8300(2) 0.8883(2) 0.40435(19) 0.0274(6) Uani 1 1 d . . . .
H2 H 0.9050 0.9368 0.4438 0.033 Uiso 0.5 1 calc R P . .
C1 C 1.2235(3) 1.0094(3) 0.3769(2) 0.0264(7) Uani 1 1 d . . . .
C2 C 1.2530(3) 0.9566(3) 0.2780(2) 0.0307(7) Uani 1 1 d . . . .
H2A H 1.3376 0.9713 0.2598 0.037 Uiso 1 1 calc R . . .
C3 C 1.1385(3) 0.8811(3) 0.2140(2) 0.0295(7) Uani 1 1 d . . . .
H3 H 1.1294 0.8335 0.1435 0.035 Uiso 1 1 calc R . . .
C4 C 1.0349(3) 0.8861(2) 0.2710(2) 0.0260(7) Uani 1 1 d . . . .
C5 C 0.9029(3) 0.8194(2) 0.2372(2) 0.0264(7) Uani 1 1 d . . . .
C6 C 0.8077(3) 0.8222(3) 0.3006(2) 0.0270(7) Uani 1 1 d . . . .
C7 C 0.6703(3) 0.7543(3) 0.2639(2) 0.0333(8) Uani 1 1 d . . . .
H7 H 0.6302 0.7019 0.1950 0.040 Uiso 1 1 calc R . . .
C8 C 0.6112(3) 0.7797(3) 0.3459(2) 0.0357(8) Uani 1 1 d . . . .
H8 H 0.5206 0.7488 0.3462 0.043 Uiso 1 1 calc R . . .
C9 C 0.7107(3) 0.8629(3) 0.4337(2) 0.0289(7) Uani 1 1 d . . . .
C10 C 0.6855(3) 0.9096(3) 0.5342(2) 0.0298(7) Uani 1 1 d . . . .
C11 C 0.8627(3) 0.7389(3) 0.1266(2) 0.0262(7) Uani 1 1 d . . . .
C12 C 0.8640(3) 0.7799(3) 0.0377(2) 0.0280(7) Uani 1 1 d . . . .
H12 H 0.8946 0.8603 0.0481 0.034 Uiso 1 1 calc R . . .
C13 C 0.8218(3) 0.7061(3) -0.0659(2) 0.0281(7) Uani 1 1 d . . . .
C14 C 0.7784(3) 0.5885(3) -0.0781(2) 0.0281(7) Uani 1 1 d . . . .
H14 H 0.7479 0.5370 -0.1483 0.034 Uiso 1 1 calc R . . .
C15 C 0.7780(3) 0.5439(3) 0.0085(2) 0.0269(7) Uani 1 1 d . . . .
C16 C 0.8212(3) 0.6211(3) 0.1109(2) 0.0271(7) Uani 1 1 d . . . .
H16 H 0.8223 0.5925 0.1713 0.032 Uiso 1 1 calc R . . .
C17 C 0.8173(3) 0.7519(3) -0.1640(2) 0.0344(7) Uani 1 1 d . . . .
C18 C 0.8348(7) 0.6641(4) -0.2604(3) 0.0815(17) Uani 1 1 d . . . .
H18A H 0.9203 0.6453 -0.2428 0.122 Uiso 1 1 calc GR . . .
H18B H 0.8334 0.6963 -0.3210 0.122 Uiso 1 1 calc GR . . .
H18C H 0.7619 0.5941 -0.2793 0.122 Uiso 1 1 calc GR . . .
C19 C 0.6800(4) 0.7741(4) -0.1921(4) 0.0668(13) Uani 1 1 d . . . .
H19A H 0.6106 0.7032 -0.2039 0.100 Uiso 1 1 calc GR . . .
H19B H 0.6723 0.7985 -0.2574 0.100 Uiso 1 1 calc GR . . .
H19C H 0.6691 0.8346 -0.1332 0.100 Uiso 1 1 calc GR . . .
C20 C 0.9249(4) 0.8618(4) -0.1425(3) 0.0540(11) Uani 1 1 d . . . .
H20A H 0.9081 0.9230 -0.0874 0.081 Uiso 1 1 calc GR . . .
H20B H 0.9240 0.8845 -0.2085 0.081 Uiso 1 1 calc GR . . .
H20C H 1.0122 0.8492 -0.1177 0.081 Uiso 1 1 calc GR . . .
C21 C 0.7346(3) 0.4144(3) -0.0046(2) 0.0310(7) Uani 1 1 d . . . .
C22 C 0.8539(3) 0.3777(3) 0.0464(3) 0.0391(8) Uani 1 1 d . . . .
H22A H 0.9262 0.3913 0.0089 0.059 Uiso 1 1 calc GR . . .
H22B H 0.8268 0.2957 0.0411 0.059 Uiso 1 1 calc GR . . .
H22C H 0.8850 0.4227 0.1219 0.059 Uiso 1 1 calc GR . . .
C23 C 0.6891(3) 0.3434(3) -0.1214(3) 0.0390(8) Uani 1 1 d . . . .
H23A H 0.6148 0.3675 -0.1564 0.059 Uiso 1 1 calc GR . . .
H23B H 0.6598 0.2617 -0.1259 0.059 Uiso 1 1 calc GR . . .
H23C H 0.7634 0.3551 -0.1573 0.059 Uiso 1 1 calc GR . . .
C24 C 0.6172(3) 0.3887(3) 0.0509(3) 0.0415(9) Uani 1 1 d . . . .
H24A H 0.6441 0.4340 0.1264 0.062 Uiso 1 1 calc GR . . .
H24B H 0.5932 0.3066 0.0457 0.062 Uiso 1 1 calc GR . . .
H24C H 0.5400 0.4093 0.0157 0.062 Uiso 1 1 calc GR . . .
C25 C 0.5527(3) 0.8697(3) 0.5489(2) 0.0341(8) Uani 1 1 d . . . .
C26 C 0.4446(3) 0.8334(3) 0.5641(3) 0.0421(9) Uani 1 1 d . . . .
C27 C 0.3133(4) 0.6408(4) 0.6362(4) 0.0653(13) Uani 1 1 d . . . .
H27 H 0.3736 0.6719 0.7091 0.078 Uiso 1 1 calc R . . .
C28 C 0.3853(5) 0.5686(4) 0.5697(4) 0.0776(14) Uani 1 1 d . . . .
H28A H 0.3297 0.5323 0.4974 0.116 Uiso 1 1 calc GR . . .
H28B H 0.4037 0.5089 0.6023 0.116 Uiso 1 1 calc GR . . .
H28C H 0.4697 0.6174 0.5661 0.116 Uiso 1 1 calc GR . . .
C29 C 0.1878(4) 0.5670(4) 0.6512(4) 0.0678(13) Uani 1 1 d . . . .
H29A H 0.1461 0.6153 0.6991 0.102 Uiso 1 1 calc GR . . .
H29B H 0.2107 0.5077 0.6825 0.102 Uiso 1 1 calc GR . . .
H29C H 0.1254 0.5302 0.5817 0.102 Uiso 1 1 calc GR . . .
C30 C 0.1474(4) 0.7460(4) 0.4826(4) 0.0560(11) Uani 1 1 d . . . .
H30 H 0.1601 0.8195 0.4625 0.067 Uiso 1 1 calc R . . .
C31 C 0.0112(4) 0.7255(4) 0.5127(4) 0.0712(14) Uani 1 1 d . . . .
H31A H -0.0081 0.6521 0.5297 0.107 Uiso 1 1 calc GR . . .
H31B H -0.0581 0.7232 0.4523 0.107 Uiso 1 1 calc GR . . .
H31C H 0.0127 0.7882 0.5751 0.107 Uiso 1 1 calc GR . . .
C32 C 0.1481(4) 0.6520(5) 0.3828(3) 0.0692(14) Uani 1 1 d . . . .
H32A H 0.2361 0.6674 0.3654 0.104 Uiso 1 1 calc GR . . .
H32B H 0.0801 0.6518 0.3225 0.104 Uiso 1 1 calc GR . . .
H32C H 0.1285 0.5769 0.3966 0.104 Uiso 1 1 calc GR . . .
N3 N 0.3050(5) 0.9276(4) 1.0151(4) 0.0500(12) Uani 0.781(6) 1 d D P A 1
C33 C 0.2596(4) 0.8817(5) 0.7125(4) 0.0420(13) Uani 0.781(6) 1 d D P A 1
H33A H 0.1999 0.9240 0.6827 0.050 Uiso 0.781(6) 1 calc R P A 1
H33B H 0.2132 0.8419 0.7578 0.050 Uiso 0.781(6) 1 calc R P A 1
C34 C 0.3867(5) 0.9679(4) 0.7823(4) 0.0382(12) Uani 0.781(6) 1 d D P A 1
H34A H 0.4249 1.0172 0.7403 0.046 Uiso 0.781(6) 1 calc R P A 1
H34B H 0.4525 0.9256 0.8021 0.046 Uiso 0.781(6) 1 calc R P A 1
C35 C 0.3643(9) 1.0449(9) 0.8848(6) 0.0446(16) Uani 0.781(6) 1 d D P A 1
H35A H 0.4466 1.1070 0.9207 0.054 Uiso 0.781(6) 1 calc R P A 1
H35B H 0.2917 1.0812 0.8659 0.054 Uiso 0.781(6) 1 calc R P A 1
C36 C 0.3293(4) 0.9790(4) 0.9581(3) 0.0368(12) Uani 0.781(6) 1 d D P A 1
N3B N 0.6141(18) 1.0772(14) 0.9394(16) 0.060(5) Uani 0.219(6) 1 d D P A 2
C33B C 0.3156(19) 0.8331(13) 0.7465(11) 0.048(3) Uani 0.219(6) 1 d D P A 2
H33C H 0.2445 0.7930 0.7753 0.057 Uiso 0.219(6) 1 calc R P A 2
H33D H 0.4036 0.8302 0.7845 0.057 Uiso 0.219(6) 1 calc R P A 2
C34B C 0.309(2) 0.9581(16) 0.7553(15) 0.048(3) Uani 0.219(6) 1 d D P A 2
H34C H 0.3636 0.9883 0.7091 0.057 Uiso 0.219(6) 1 calc R P A 2
H34D H 0.2155 0.9587 0.7288 0.057 Uiso 0.219(6) 1 calc R P A 2
C35B C 0.359(3) 1.037(3) 0.870(3) 0.048(3) Uani 0.219(6) 1 d D P A 2
H35C H 0.3327 1.1100 0.8740 0.057 Uiso 0.219(6) 1 calc R P A 2
H35D H 0.3150 1.0000 0.9180 0.057 Uiso 0.219(6) 1 calc R P A 2
C36B C 0.5025(17) 1.0632(15) 0.9077(14) 0.048(3) Uani 0.219(6) 1 d D P A 2
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -2 -5 0.1317
0 -1 1 0.0085
0 1 -1 0.0085
-5 2 0 0.0601
5 -3 -1 0.1834
5 0 3 0.0829
-5 3 1 0.0708
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
C26 Si1 C27 106.68(18) . .
C26 Si1 C30 108.70(17) . .
C26 Si1 C33 107.13(18) . .
C26 Si1 C33B 104.6(6) . .
C27 Si1 C30 117.1(2) . .
C27 Si1 C33 111.7(2) . .
C27 Si1 C33B 82.5(5) . .
C30 Si1 C33 105.2(2) . .
C30 Si1 C33B 133.1(6) . .
C1 N1 H1 125.2 . .
C1 N1 C4 109.6(2) . .
C4 N1 H1 125.2 . .
C6 N2 H2 127.3 . .
C9 N2 H2 127.3 . .
C9 N2 C6 105.4(2) . .
N1 C1 C2 107.4(2) . .
N1 C1 C10 126.4(3) . 2_776
C10 C1 C2 126.2(3) 2_776 .
C1 C2 H2A 126.0 . .
C3 C2 C1 107.9(3) . .
C3 C2 H2A 126.0 . .
C2 C3 H3 126.0 . .
C2 C3 C4 108.1(3) . .
C4 C3 H3 126.0 . .
N1 C4 C3 106.9(2) . .
N1 C4 C5 125.8(3) . .
C5 C4 C3 127.2(3) . .
C4 C5 C6 124.4(3) . .
C4 C5 C11 117.0(2) . .
C6 C5 C11 118.5(2) . .
N2 C6 C5 125.6(3) . .
N2 C6 C7 110.4(2) . .
C5 C6 C7 124.0(3) . .
C6 C7 H7 126.7 . .
C8 C7 C6 106.7(3) . .
C8 C7 H7 126.7 . .
C7 C8 H8 126.5 . .
C7 C8 C9 107.1(3) . .
C9 C8 H8 126.5 . .
N2 C9 C8 110.5(2) . .
N2 C9 C10 126.0(3) . .
C10 C9 C8 123.5(3) . .
C1 C10 C9 126.9(3) 2_776 .
C1 C10 C25 116.1(3) 2_776 .
C9 C10 C25 117.0(3) . .
C12 C11 C5 121.1(3) . .
C16 C11 C5 120.0(3) . .
C16 C11 C12 118.9(3) . .
C11 C12 H12 119.2 . .
C13 C12 C11 121.6(3) . .
C13 C12 H12 119.2 . .
C12 C13 C14 117.6(3) . .
C12 C13 C17 121.5(3) . .
C14 C13 C17 120.8(3) . .
C13 C14 H14 118.7 . .
C15 C14 C13 122.6(3) . .
C15 C14 H14 118.7 . .
C14 C15 C16 117.8(3) . .
C14 C15 C21 122.7(3) . .
C16 C15 C21 119.5(3) . .
C11 C16 C15 121.5(3) . .
C11 C16 H16 119.3 . .
C15 C16 H16 119.3 . .
C18 C17 C13 111.4(3) . .
C18 C17 C19 108.0(4) . .
C19 C17 C13 107.7(3) . .
C20 C17 C13 111.9(3) . .
C20 C17 C18 108.0(3) . .
C20 C17 C19 109.8(3) . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18B 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C17 C20 H20A 109.5 . .
C17 C20 H20B 109.5 . .
C17 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C15 C21 C24 109.9(2) . .
C22 C21 C15 108.5(2) . .
C22 C21 C24 110.1(3) . .
C23 C21 C15 112.3(3) . .
C23 C21 C22 108.1(3) . .
C23 C21 C24 108.0(3) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22B 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23B 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C21 C24 H24A 109.5 . .
C21 C24 H24B 109.5 . .
C21 C24 H24C 109.5 . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C26 C25 C10 176.8(4) . .
C25 C26 Si1 173.3(4) . .
Si1 C27 H27 105.0 . .
C28 C27 Si1 115.7(3) . .
C28 C27 H27 105.0 . .
C28 C27 C29 111.0(4) . .
C29 C27 Si1 113.9(3) . .
C29 C27 H27 105.0 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
Si1 C30 H30 106.3 . .
C31 C30 Si1 112.9(3) . .
C31 C30 H30 106.3 . .
C32 C30 Si1 113.2(3) . .
C32 C30 H30 106.3 . .
C32 C30 C31 111.3(4) . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
Si1 C33 H33A 108.7 . .
Si1 C33 H33B 108.7 . .
H33A C33 H33B 107.6 . .
C34 C33 Si1 114.0(3) . .
C34 C33 H33A 108.7 . .
C34 C33 H33B 108.7 . .
C33 C34 H34A 108.9 . .
C33 C34 H34B 108.9 . .
C33 C34 C35 113.2(5) . .
H34A C34 H34B 107.8 . .
C35 C34 H34A 108.9 . .
C35 C34 H34B 108.9 . .
C34 C35 H35A 109.4 . .
C34 C35 H35B 109.4 . .
H35A C35 H35B 108.0 . .
C36 C35 C34 111.3(7) . .
C36 C35 H35A 109.4 . .
C36 C35 H35B 109.4 . .
N3 C36 C35 178.5(6) . .
Si1 C33B H33C 111.4 . .
Si1 C33B H33D 111.4 . .
H33C C33B H33D 109.2 . .
C34B C33B Si1 102.0(11) . .
C34B C33B H33C 111.4 . .
C34B C33B H33D 111.4 . .
C33B C34B H34C 109.1 . .
C33B C34B H34D 109.1 . .
H34C C34B H34D 107.8 . .
C35B C34B C33B 112.6(19) . .
C35B C34B H34C 109.1 . .
C35B C34B H34D 109.1 . .
C34B C35B H35C 108.9 . .
C34B C35B H35D 108.9 . .
H35C C35B H35D 107.7 . .
C36B C35B C34B 113(2) . .
C36B C35B H35C 108.9 . .
C36B C35B H35D 108.9 . .
N3B C36B C35B 175(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C26 1.838(3) .
Si1 C27 1.840(5) .
Si1 C30 1.860(4) .
Si1 C33 1.912(5) .
Si1 C33B 1.892(13) .
N1 H1 0.8800 .
N1 C1 1.365(4) .
N1 C4 1.380(4) .
N2 H2 0.8800 .
N2 C6 1.369(4) .
N2 C9 1.368(4) .
C1 C2 1.424(4) .
C1 C10 1.403(4) 2_776
C2 H2A 0.9500 .
C2 C3 1.364(4) .
C3 H3 0.9500 .
C3 C4 1.422(4) .
C4 C5 1.397(4) .
C5 C6 1.404(4) .
C5 C11 1.490(4) .
C6 C7 1.450(4) .
C7 H7 0.9500 .
C7 C8 1.337(4) .
C8 H8 0.9500 .
C8 C9 1.443(4) .
C9 C10 1.404(4) .
C10 C1 1.403(4) 2_776
C10 C25 1.441(4) .
C11 C12 1.393(4) .
C11 C16 1.388(4) .
C12 H12 0.9500 .
C12 C13 1.390(4) .
C13 C14 1.395(4) .
C13 C17 1.538(4) .
C14 H14 0.9500 .
C14 C15 1.390(4) .
C15 C16 1.394(4) .
C15 C21 1.533(4) .
C16 H16 0.9500 .
C17 C18 1.522(5) .
C17 C19 1.527(5) .
C17 C20 1.512(5) .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 C22 1.531(5) .
C21 C23 1.520(4) .
C21 C24 1.550(4) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 C26 1.199(4) .
C27 H27 1.0000 .
C27 C28 1.500(7) .
C27 C29 1.514(6) .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 H30 1.0000 .
C30 C31 1.532(5) .
C30 C32 1.532(6) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
N3 C36 1.129(6) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C33 C34 1.519(6) .
C34 H34A 0.9900 .
C34 H34B 0.9900 .
C34 C35 1.537(7) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C35 C36 1.456(15) .
N3B C36B 1.141(16) .
C33B H33C 0.9900 .
C33B H33D 0.9900 .
C33B C34B 1.542(16) .
C34B H34C 0.9900 .
C34B H34D 0.9900 .
C34B C35B 1.528(17) .
C35B H35C 0.9900 .
C35B H35D 0.9900 .
C35B C36B 1.45(2) .
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_4
Si1 C33 C34 C35 -170.3(6) . .
Si1 C33B C34B C35B -167(2) . .
N1 C1 C2 C3 -0.8(4) . .
N1 C4 C5 C6 -1.4(5) . .
N1 C4 C5 C11 179.6(3) . .
N2 C6 C7 C8 -0.2(4) . .
N2 C9 C10 C1 0.1(6) . 2_776
N2 C9 C10 C25 -179.2(3) . .
C1 N1 C4 C3 -0.4(3) . .
C1 N1 C4 C5 176.5(3) . .
C1 C2 C3 C4 0.6(4) . .
C2 C3 C4 N1 -0.1(4) . .
C2 C3 C4 C5 -177.0(3) . .
C3 C4 C5 C6 174.9(3) . .
C3 C4 C5 C11 -4.1(5) . .
C4 N1 C1 C2 0.8(3) . .
C4 N1 C1 C10 -178.5(3) . 2_776
C4 C5 C6 N2 -1.2(5) . .
C4 C5 C6 C7 178.8(3) . .
C4 C5 C11 C12 -63.3(4) . .
C4 C5 C11 C16 117.6(3) . .
C5 C6 C7 C8 179.8(3) . .
C5 C11 C12 C13 -177.4(3) . .
C5 C11 C16 C15 177.5(3) . .
C6 N2 C9 C8 -0.5(4) . .
C6 N2 C9 C10 179.5(3) . .
C6 C5 C11 C12 117.6(3) . .
C6 C5 C11 C16 -61.5(4) . .
C6 C7 C8 C9 -0.1(4) . .
C7 C8 C9 N2 0.4(4) . .
C7 C8 C9 C10 -179.6(3) . .
C8 C9 C10 C1 -179.9(3) . 2_776
C8 C9 C10 C25 0.9(5) . .
C9 N2 C6 C5 -179.6(3) . .
C9 N2 C6 C7 0.4(3) . .
C10 C1 C2 C3 178.4(3) 2_776 .
C11 C5 C6 N2 177.8(3) . .
C11 C5 C6 C7 -2.2(5) . .
C11 C12 C13 C14 -0.4(4) . .
C11 C12 C13 C17 177.2(3) . .
C12 C11 C16 C15 -1.6(4) . .
C12 C13 C14 C15 -1.0(4) . .
C12 C13 C17 C18 152.4(4) . .
C12 C13 C17 C19 -89.3(4) . .
C12 C13 C17 C20 31.4(4) . .
C13 C14 C15 C16 1.0(4) . .
C13 C14 C15 C21 -178.0(3) . .
C14 C13 C17 C18 -30.1(5) . .
C14 C13 C17 C19 88.1(4) . .
C14 C13 C17 C20 -151.1(3) . .
C14 C15 C16 C11 0.4(4) . .
C14 C15 C21 C22 117.7(3) . .
C14 C15 C21 C23 -1.7(4) . .
C14 C15 C21 C24 -122.0(3) . .
C16 C11 C12 C13 1.6(4) . .
C16 C15 C21 C22 -61.3(3) . .
C16 C15 C21 C23 179.3(3) . .
C16 C15 C21 C24 59.1(4) . .
C17 C13 C14 C15 -178.5(3) . .
C21 C15 C16 C11 179.4(2) . .
C26 Si1 C27 C28 -41.3(4) . .
C26 Si1 C27 C29 -171.9(3) . .
C26 Si1 C30 C31 -163.5(3) . .
C26 Si1 C30 C32 68.9(3) . .
C26 Si1 C33B C34B 72.1(13) . .
C27 Si1 C30 C31 75.6(4) . .
C27 Si1 C30 C32 -52.0(3) . .
C27 Si1 C33B C34B 177.5(13) . .
C30 Si1 C27 C28 80.6(4) . .
C30 Si1 C27 C29 -49.9(4) . .
C30 Si1 C33B C34B -62.1(15) . .
C33 Si1 C27 C28 -158.1(3) . .
C33 Si1 C27 C29 71.4(4) . .
C33 Si1 C30 C31 -49.1(4) . .
C33 Si1 C30 C32 -176.6(3) . .
C33 C34 C35 C36 68.2(7) . .
C33B Si1 C27 C28 -144.4(7) . .
C33B Si1 C27 C29 85.1(7) . .
C33B Si1 C30 C31 -30.6(8) . .
C33B Si1 C30 C32 -158.2(7) . .
C33B C34B C35B C36B 72(4) . .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9992 -1.9966 -4.9834 -0.2644 -0.1435 -0.2064
0.0009 -0.9973 0.9980 -0.0250 0.0641 0.0136
-0.0009 0.9973 -0.9980 0.0250 -0.0641 -0.0136
-4.9863 1.9889 0.0034 0.1099 0.0432 -0.3218
4.9861 -2.9864 -0.9998 -0.1961 -0.0618 0.2881
4.9872 0.0063 2.9867 0.0931 0.0353 0.4126
-4.9861 2.9864 0.9998 0.1961 0.0618 -0.2881
