#------------------------------------------------------------------------------
#$Date: 2020-07-06 06:11:01 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253907 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/43/7704340.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_7704340
loop_
_publ_author_name
'Vanga, Mukundam'
'Sa, Shreenibasa'
'Kumari, Anupa'
'Murali, Anna Chandrasekar'
'Nayak, Prakash'
'Das, Ritwick'
'Venkatasubbaiah, Krishnan'
_publ_section_title
;
 Synthesis of π-extended B ← N coordinated phenanthroimidazole
 dimers and their linear and nonlinear optical properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7737
_journal_page_last               7746
_journal_paper_doi               10.1039/d0dt01024c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C83 H76 B2 N4'
_chemical_formula_sum            'C83 H76 B2 N4'
_chemical_formula_weight         1151.09
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-08-06 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                103.453(4)
_cell_angle_beta                 115.561(4)
_cell_angle_gamma                105.550(3)
_cell_formula_units_Z            2
_cell_length_a                   15.4087(5)
_cell_length_b                   16.2830(6)
_cell_length_c                   16.8471(8)
_cell_measurement_reflns_used    6822
_cell_measurement_temperature    293.6(2)
_cell_measurement_theta_max      70.1380
_cell_measurement_theta_min      4.3390
_cell_volume                     3365.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.6(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     85.00 118.00   0.50    8.00    --   97.23  45.00  60.00   66
  2  ω    119.00 148.00   0.50    8.00    --   97.23  45.00  60.00   58
  3  ω     89.00 155.00   0.50    8.00    --   97.23  45.00  30.00  132
  4  ω     93.00 176.00   0.50    8.00    --   97.23  30.00  90.00  166
  5  ω     84.00 172.00   0.50    8.00    --   97.23  45.00 150.00  176
  6  ω     85.00 166.00   0.50    8.00    --   97.23  61.00 120.00  162
  7  ω    -10.00  42.00   0.50    2.00    --    0.00  57.00 -30.00  104
  8  ω    -11.00  76.00   0.50    2.00    --    0.00  38.00 -90.00  174
  9  ω    141.00 172.00   0.50    8.00    --   97.23 125.00 -90.00   62
 10  ω      0.00  46.00   0.50    2.00    --    0.00  77.00  90.00   92
 11  ω    -75.00 -50.00   0.50    2.00    --    0.00 -38.00-120.00   50
 12  ω     24.00 108.00   0.50    8.00    --   97.23 -95.00-150.00  168
 13  ω     90.00 117.00   0.50    8.00    --   97.23-125.00-120.00   54
 14  ω     31.00  57.00   0.50    8.00    --   97.23-125.00-120.00   52
 15  ω     53.00 104.00   0.50    8.00    --   97.23 -95.00  30.00  102
 16  ω     32.00  59.00   0.50    8.00    --   97.23-125.00  60.00   54
 17  ω     76.00 122.00   0.50    8.00    --   97.23-125.00  60.00   92
 18  ω     35.00 108.00   0.50    8.00    --   97.23 -95.00  90.00  146
 19  ω     34.00  97.00   0.50    8.00    --   97.23 -95.00 -60.00  126
 20  ω    -56.00  23.00   0.50    2.00    --    0.00 -77.00 150.00  158
 21  ω    -99.00 -61.00   0.50    8.00    --  -86.25  45.00 -30.00   76
 22  ω    -50.00 -16.00   0.50    8.00    --  -86.25  61.00-150.00   68
 23  ω    -99.00 -72.00   0.50    8.00    --  -86.25  61.00-150.00   54
 24  ω     31.00 114.00   0.50    8.00    --   97.23 -61.00 150.00  166
 25  ω    -17.00  12.00   0.50    2.00    --    0.00 -38.00-120.00   58
 26  ω     19.00  99.00   0.50    8.00    --   97.23 -15.00-180.00  160
 27  ω     25.00  92.00   0.50    8.00    --   97.23 -77.00 -60.00  134
 28  ω     23.00  92.00   0.50    8.00    --   97.23 -45.00 -30.00  138
 29  ω     30.00  96.00   0.50    8.00    --   97.23 -77.00  90.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0708454000
_diffrn_orient_matrix_UB_12      0.0478271000
_diffrn_orient_matrix_UB_13      -0.0329192000
_diffrn_orient_matrix_UB_21      0.0973221000
_diffrn_orient_matrix_UB_22      0.0400672000
_diffrn_orient_matrix_UB_23      0.1025113000
_diffrn_orient_matrix_UB_31      0.0205428000
_diffrn_orient_matrix_UB_32      -0.0871620000
_diffrn_orient_matrix_UB_33      -0.0254717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33325
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_min         4.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9d (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         12279
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1516P)²+1.0681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2417
_refine_ls_wR_factor_ref         0.2715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7761
_reflns_number_total             12279
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01024c2.cif
_cod_data_source_block           sample1
_cod_depositor_comments
'Adding full bibliography for 7704339--7704342.cif.'
_cod_database_code               7704340
_chemical_oxdiff_formula         'C85 H76 N4'
_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.
;
_diffrn_oxdiff_ac3_digest_frames
;
01f53c4c4b49d8989220ef9bdd2f50de3f03180a807
;
_diffrn_oxdiff_ac3_digest_hkl
;
01f228e01f4658ae3cbd1c05f1277eb3347fb4
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C68-C67 \\sim C74-C67 \\sim C69-C68 \\sim C75-C74 \\sim C69-C70 \\sim C76-C75
\\sim C71-C70 \\sim C76-C77
 \\sim C71-C72 \\sim C78-C77 \\sim C73-C72 \\sim C78-C79
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C76 \\sim C77 \\sim C78 \\sim C79 \\sim C70 \\sim C71 \\sim C72 \\sim C73:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C69(H69A,H69B), C76(H76A,H76B), C70(H70A,H70B), C72(H72A,
 H72B), C77(H77A,H77B), C78(H78A,H78B), C71(H71A,H71B)
4.b Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C79(H79A,H79B,H79C), C73(H73A,H73B,H73C)
;
_shelx_shelxl_version_number     2016/4
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.231
_oxdiff_exptl_absorpt_empirical_full_min 0.485
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
N1 N -0.34872(18) -0.08022(17) 0.26567(18) 0.0641(6) Uani 1 1 d . . . . .
N4 N 1.08327(19) 0.90979(17) 1.07600(18) 0.0647(6) Uani 1 1 d . . . . .
N3 N 1.17911(19) 0.89246(17) 1.01175(19) 0.0665(7) Uani 1 1 d . . . . .
N2 N -0.29607(19) 0.04850(17) 0.38701(19) 0.0666(7) Uani 1 1 d . . . . .
C31 C 0.4012(2) 0.29955(19) 0.6380(2) 0.0611(7) Uani 1 1 d . . . . .
C30 C 0.3586(2) 0.2039(2) 0.5907(2) 0.0617(7) Uani 1 1 d . . . . .
C1 C -0.2657(2) -0.0007(2) 0.3386(2) 0.0635(7) Uani 1 1 d . . . . .
C28 C 0.1820(2) 0.1979(2) 0.5342(2) 0.0626(7) Uani 1 1 d . . . . .
C32 C 0.3366(2) 0.3450(2) 0.6380(2) 0.0644(8) Uani 1 1 d . . . . .
C34 C 0.5116(2) 0.3697(2) 0.6928(2) 0.0647(8) Uani 1 1 d . . . . .
C16 C -0.3449(2) -0.1425(2) 0.1916(2) 0.0630(7) Uani 1 1 d . . . . .
C61 C 1.1955(2) 0.8551(2) 0.9359(2) 0.0641(8) Uani 1 1 d . . . . .
C25 C 0.0650(2) 0.1428(2) 0.4787(2) 0.0644(8) Uani 1 1 d . . . . .
C22 C -0.1528(2) 0.0394(2) 0.3756(2) 0.0622(7) Uani 1 1 d . . . . .
C3 C -0.4380(2) -0.0813(2) 0.2696(2) 0.0635(7) Uani 1 1 d . . . . .
C39 C 0.5136(2) 0.4561(2) 0.7280(2) 0.0653(8) Uani 1 1 d . . . . .
C33 C 0.2277(2) 0.2946(2) 0.5849(2) 0.0655(8) Uani 1 1 d . . . . .
C24 C 0.0166(2) 0.0610(2) 0.3976(3) 0.0705(8) Uani 1 1 d . . . . .
C26 C 0.0017(2) 0.1717(2) 0.5072(2) 0.0667(8) Uani 1 1 d . . . . .
C46 C 1.0877(2) 0.8537(2) 1.0080(2) 0.0646(8) Uani 1 1 d . . . . .
C27 C -0.1075(2) 0.1219(2) 0.4569(2) 0.0642(7) Uani 1 1 d . . . . .
C2 C -0.4045(2) -0.0010(2) 0.3444(2) 0.0653(8) Uani 1 1 d . . . . .
C29 C 0.2497(2) 0.1537(2) 0.5394(2) 0.0642(7) Uani 1 1 d . . . . .
C38 C 0.6096(2) 0.5350(2) 0.7813(2) 0.0697(8) Uani 1 1 d . . . . .
C47 C 1.2378(2) 0.9807(2) 1.0879(2) 0.0648(8) Uani 1 1 d . . . . .
C4 C -0.5442(2) -0.1540(2) 0.2156(2) 0.0682(8) Uani 1 1 d . . . . .
C37 C 0.7034(2) 0.5263(2) 0.7983(2) 0.0719(8) Uani 1 1 d . . . . .
C60 C 1.1759(2) 0.9908(2) 1.1257(2) 0.0648(8) Uani 1 1 d . . . . .
C35 C 0.6039(2) 0.3597(2) 0.7097(3) 0.0718(9) Uani 1 1 d . . . . .
C23 C -0.0918(2) 0.0089(2) 0.3455(3) 0.0697(9) Uani 1 1 d . . . . .
C45 C 0.8313(2) 0.6846(2) 0.9303(2) 0.0696(8) Uani 1 1 d . . . . .
C43 C 0.9965(2) 0.7644(2) 0.9479(2) 0.0674(8) Uani 1 1 d . . . . .
C44 C 0.9270(2) 0.7642(2) 0.9806(2) 0.0646(7) Uani 1 1 d . . . . .
C15 C -0.4765(2) 0.0210(2) 0.3683(2) 0.0702(8) Uani 1 1 d . . . . .
C67 C 0.4025(2) 0.44988(19) 0.6988(2) 0.0687(8) Uani 1 1 d D . . . .
C10 C -0.5836(2) -0.0453(3) 0.3130(3) 0.0731(9) Uani 1 1 d . . . . .
C40 C 0.8065(2) 0.6097(2) 0.8531(2) 0.0721(8) Uani 1 1 d . . . . .
C9 C -0.6172(2) -0.1344(2) 0.2371(3) 0.0713(8) Uani 1 1 d . . . . .
C36 C 0.6985(3) 0.4379(2) 0.7615(3) 0.0764(9) Uani 1 1 d . . . . .
C82 C 1.0013(3) 0.8405(3) 1.1684(3) 0.0851(10) Uani 1 1 d . . . . .
H82A H 1.039619 0.802219 1.173542 0.128 Uiso 1 1 calc GR . . . .
H82B H 0.937295 0.809612 1.166283 0.128 Uiso 1 1 calc GR . . . .
H82C H 1.044370 0.898973 1.223083 0.128 Uiso 1 1 calc GR . . . .
C59 C 1.2052(3) 1.0765(2) 1.1981(2) 0.0739(9) Uani 1 1 d . . . . .
C5 C -0.5772(3) -0.2421(2) 0.1476(3) 0.0794(10) Uani 1 1 d . . . . .
C48 C 1.3413(3) 1.0490(2) 1.1257(3) 0.0759(9) Uani 1 1 d . . . . .
C66 C 1.2503(3) 0.8005(3) 0.9432(3) 0.0847(10) Uani 1 1 d . . . . .
C21 C -0.3088(3) -0.2086(3) 0.2088(3) 0.0825(10) Uani 1 1 d . . . . .
C74 C 0.3974(3) 0.4812(3) 0.7900(3) 0.0827(10) Uani 1 1 d D . . . .
C62 C 1.1489(3) 0.8693(3) 0.8537(3) 0.0872(10) Uani 1 1 d . . . . .
C8 C -0.7222(3) -0.2032(3) 0.1861(3) 0.0855(11) Uani 1 1 d . . . . .
C6 C -0.6787(3) -0.3077(3) 0.1023(3) 0.0889(11) Uani 1 1 d . . . . .
C53 C 1.3733(3) 1.1344(2) 1.1994(3) 0.0844(10) Uani 1 1 d . . . . .
C41 C 0.8805(3) 0.6129(3) 0.8256(3) 0.0839(11) Uani 1 1 d . . . . .
C68 C 0.3733(3) 0.5085(2) 0.6412(3) 0.0853(11) Uani 1 1 d D . . . .
C42 C 0.9756(3) 0.6898(2) 0.8719(3) 0.0816(10) Uani 1 1 d . . . . .
C54 C 1.3033(3) 1.1502(2) 1.2314(3) 0.0857(10) Uani 1 1 d . . . . .
C14 C -0.4453(3) 0.1053(3) 0.4398(3) 0.0895(11) Uani 1 1 d . . . . .
C7 C -0.7520(3) -0.2880(3) 0.1200(3) 0.0926(12) Uani 1 1 d . . . . .
C58 C 1.1417(4) 1.0925(3) 1.2343(3) 0.0907(11) Uani 1 1 d . . . . .
C83 C 0.8988(3) 0.9139(3) 1.0493(3) 0.0884(11) Uani 1 1 d . . . . .
H83A H 0.919770 0.961511 1.108286 0.133 Uiso 1 1 calc GR . . . .
H83B H 0.826016 0.871621 1.019055 0.133 Uiso 1 1 calc GR . . . .
H83C H 0.906878 0.941994 1.007306 0.133 Uiso 1 1 calc GR . . . .
C80 C -0.1754(3) 0.1413(3) 0.5786(3) 0.0898(11) Uani 1 1 d . . . . .
H80A H -0.227014 0.156066 0.588882 0.135 Uiso 1 1 calc GR . . . .
H80B H -0.105514 0.186323 0.629683 0.135 Uiso 1 1 calc GR . . . .
H80C H -0.183172 0.080449 0.577415 0.135 Uiso 1 1 calc GR . . . .
C11 C -0.6543(3) -0.0227(3) 0.3352(3) 0.0879(11) Uani 1 1 d . . . . .
C17 C -0.3795(4) -0.1355(3) 0.1057(3) 0.0919(11) Uani 1 1 d . . . . .
C49 C 1.4112(3) 1.0354(3) 1.0984(4) 0.0918(12) Uani 1 1 d . . . . .
C81 C -0.2018(3) 0.2353(3) 0.4630(3) 0.0905(11) Uani 1 1 d . . . . .
H81A H -0.221391 0.227291 0.398383 0.136 Uiso 1 1 calc GR . . . .
H81B H -0.134531 0.287732 0.507200 0.136 Uiso 1 1 calc GR . . . .
H81C H -0.254576 0.245764 0.474342 0.136 Uiso 1 1 calc GR . . . .
C65 C 1.2560(4) 0.7579(3) 0.8650(4) 0.1013(14) Uani 1 1 d . . . . .
C12 C -0.6226(3) 0.0605(4) 0.4046(3) 0.1031(14) Uani 1 1 d . . . . .
C64 C 1.2089(4) 0.7715(3) 0.7824(4) 0.1042(14) Uani 1 1 d . . . . .
B2 B 0.9722(3) 0.8582(2) 1.0718(3) 0.0662(9) Uani 1 1 d . . . . .
B1 B -0.1931(3) 0.1430(3) 0.4780(3) 0.0682(9) Uani 1 1 d . . . . .
C20 C -0.3084(4) -0.2681(3) 0.1360(5) 0.1041(14) Uani 1 1 d . . . . .
C75 C 0.2897(3) 0.4694(3) 0.7757(3) 0.1075(14) Uani 1 1 d D . . . .
H75A H 0.260940 0.500605 0.735183 0.129 Uiso 1 1 calc R . . . .
H75B H 0.242361 0.403706 0.741692 0.129 Uiso 1 1 calc R . . . .
C50 C 1.5122(3) 1.1027(3) 1.1422(4) 0.1124(15) Uani 1 1 d . . . . .
C63 C 1.1562(4) 0.8259(4) 0.7764(4) 0.1068(14) Uani 1 1 d . . . . .
C13 C -0.5185(3) 0.1254(4) 0.4572(3) 0.1050(14) Uani 1 1 d . . . . .
C52 C 1.4775(4) 1.2018(3) 1.2417(4) 0.1082(15) Uani 1 1 d . . . . .
C19 C -0.3447(4) -0.2631(4) 0.0492(5) 0.1153(17) Uani 1 1 d . . . . .
C69 C 0.3774(4) 0.4845(3) 0.5516(3) 0.1037(13) Uani 1 1 d D . . . .
H69A H 0.332463 0.418812 0.512146 0.124 Uiso 1 1 calc R . . . .
H69B H 0.449405 0.494029 0.569894 0.124 Uiso 1 1 calc R . . . .
C18 C -0.3784(5) -0.1966(4) 0.0331(4) 0.1180(17) Uani 1 1 d . . . . .
C57 C 1.1696(5) 1.1777(3) 1.2982(4) 0.1183(16) Uani 1 1 d . . . . .
C55 C 1.3290(5) 1.2371(3) 1.2965(4) 0.1209(18) Uani 1 1 d . . . . .
C51 C 1.5443(4) 1.1866(4) 1.2147(4) 0.1214(18) Uani 1 1 d . . . . .
C56 C 1.2636(5) 1.2506(4) 1.3280(4) 0.136(2) Uani 1 1 d . . . . .
C76 C 0.2907(4) 0.5065(4) 0.8668(4) 0.148(2) Uani 1 1 d D U . . .
H76A H 0.343942 0.570247 0.905120 0.177 Uiso 1 1 calc R . . . .
H76B H 0.309634 0.469850 0.903831 0.177 Uiso 1 1 calc R . . . .
C70 C 0.3440(5) 0.5382(4) 0.4911(4) 0.147(2) Uani 1 1 d D U . . .
H70A H 0.395341 0.602707 0.527030 0.176 Uiso 1 1 calc R . . . .
H70B H 0.346463 0.514183 0.434084 0.176 Uiso 1 1 calc R . . . .
C72 C 0.1465(6) 0.4438(5) 0.4182(5) 0.184(3) Uani 1 1 d D U . . .
H72A H 0.160279 0.414786 0.463874 0.220 Uiso 1 1 calc R . . . .
H72B H 0.139021 0.403301 0.361156 0.220 Uiso 1 1 calc R . . . .
C77 C 0.1824(6) 0.5035(7) 0.8456(7) 0.236(5) Uani 1 1 d D U . . .
H77A H 0.193246 0.559017 0.892425 0.284 Uiso 1 1 calc R . . . .
H77B H 0.144834 0.504356 0.782717 0.284 Uiso 1 1 calc R . . . .
C79 C 0.0126(8) 0.4204(7) 0.8337(12) 0.305(7) Uani 1 1 d D U . . .
H79A H 0.022342 0.452063 0.894617 0.458 Uiso 1 1 calc GR . . . .
H79B H -0.037618 0.356802 0.805787 0.458 Uiso 1 1 calc GR . . . .
H79C H -0.013440 0.450371 0.791662 0.458 Uiso 1 1 calc GR . . . .
C78 C 0.1178(8) 0.4234(8) 0.8479(12) 0.309(6) Uani 1 1 d D U . . .
H78A H 0.157894 0.420401 0.909258 0.371 Uiso 1 1 calc R . . . .
H78B H 0.103735 0.368253 0.798328 0.371 Uiso 1 1 calc R . . . .
C73 C 0.0445(7) 0.4550(9) 0.3920(10) 0.308(7) Uani 1 1 d D U . . .
H73A H -0.014458 0.395003 0.354318 0.463 Uiso 1 1 calc GR . . . .
H73B H 0.036884 0.492849 0.355626 0.463 Uiso 1 1 calc GR . . . .
H73C H 0.046439 0.484432 0.449600 0.463 Uiso 1 1 calc GR . . . .
C71 C 0.2370(5) 0.5350(4) 0.4607(5) 0.152(2) Uani 1 1 d D U . . .
H71A H 0.220181 0.563011 0.414254 0.182 Uiso 1 1 calc R . . . .
H71B H 0.241199 0.574490 0.516299 0.182 Uiso 1 1 calc R . . . .
H26 H 0.042(3) 0.230(2) 0.567(3) 0.079(10) Uiso 1 1 d . . . . .
H35 H 0.601(3) 0.293(3) 0.677(3) 0.086(10) Uiso 1 1 d . . . . .
H8 H -0.777(3) -0.192(2) 0.198(2) 0.071(9) Uiso 1 1 d . . . . .
H45 H 0.780(3) 0.687(2) 0.951(2) 0.070(9) Uiso 1 1 d . . . . .
H38 H 0.615(3) 0.600(3) 0.803(3) 0.098(12) Uiso 1 1 d . . . . .
H24 H 0.062(3) 0.044(3) 0.375(3) 0.092(11) Uiso 1 1 d . . . . .
H33 H 0.185(3) 0.328(2) 0.581(2) 0.072(9) Uiso 1 1 d . . . . .
H29 H 0.217(3) 0.080(2) 0.512(2) 0.080(10) Uiso 1 1 d . . . . .
H23 H -0.124(2) -0.043(2) 0.294(2) 0.059(8) Uiso 1 1 d . . . . .
H11 H -0.726(3) -0.067(2) 0.301(3) 0.080(10) Uiso 1 1 d . . . . .
H50 H 1.558(4) 1.087(3) 1.119(3) 0.112(15) Uiso 1 1 d . . . . .
H5 H -0.527(3) -0.259(3) 0.133(3) 0.089(11) Uiso 1 1 d . . . . .
H30 H 0.411(2) 0.177(2) 0.595(2) 0.063(8) Uiso 1 1 d . . . . .
H14 H -0.376(4) 0.154(3) 0.474(3) 0.107(14) Uiso 1 1 d . . . . .
H49 H 1.397(3) 0.987(3) 1.053(3) 0.085(13) Uiso 1 1 d . . . . .
H7 H -0.823(4) -0.337(3) 0.089(3) 0.116(14) Uiso 1 1 d . . . . .
H42 H 1.026(3) 0.686(3) 0.856(3) 0.089(11) Uiso 1 1 d . . . . .
H66 H 1.284(3) 0.794(2) 1.009(3) 0.081(10) Uiso 1 1 d . . . . .
H12 H -0.677(4) 0.073(3) 0.410(3) 0.113(14) Uiso 1 1 d . . . . .
H41 H 0.871(3) 0.563(2) 0.777(3) 0.080(10) Uiso 1 1 d . . . . .
H36 H 0.772(3) 0.434(2) 0.777(3) 0.090(11) Uiso 1 1 d . . . . .
H6 H -0.702(4) -0.368(3) 0.060(3) 0.115(15) Uiso 1 1 d . . . . .
H62 H 1.115(3) 0.917(3) 0.851(3) 0.116(14) Uiso 1 1 d . . . . .
H21 H -0.287(3) -0.210(3) 0.270(3) 0.089(12) Uiso 1 1 d . . . . .
H13 H -0.495(4) 0.196(4) 0.503(4) 0.137(17) Uiso 1 1 d . . . . .
H58 H 1.080(4) 1.042(3) 1.211(3) 0.122(16) Uiso 1 1 d . . . . .
H17 H -0.405(4) -0.090(4) 0.093(4) 0.15(2) Uiso 1 1 d . . . . .
H51 H 1.616(4) 1.235(4) 1.243(4) 0.134(16) Uiso 1 1 d . . . . .
H74A H 0.420(3) 0.444(2) 0.828(2) 0.076(10) Uiso 1 1 d . . . . .
H74B H 0.446(4) 0.558(3) 0.833(3) 0.119(14) Uiso 1 1 d . . . . .
H68A H 0.300(3) 0.506(2) 0.625(3) 0.090(11) Uiso 1 1 d . . . . .
H68B H 0.418(3) 0.579(3) 0.683(3) 0.094(11) Uiso 1 1 d . . . . .
H55 H 1.400(5) 1.292(4) 1.320(4) 0.16(2) Uiso 1 1 d . . . . .
H19 H -0.333(4) -0.301(3) -0.001(4) 0.132(16) Uiso 1 1 d . . . . .
H65 H 1.299(4) 0.718(4) 0.873(4) 0.140(17) Uiso 1 1 d . . . . .
H57 H 1.114(5) 1.187(4) 1.319(4) 0.16(2) Uiso 1 1 d . . . . .
H20 H -0.284(4) -0.310(4) 0.153(4) 0.126(18) Uiso 1 1 d . . . . .
H63 H 1.116(3) 0.833(3) 0.720(3) 0.104(14) Uiso 1 1 d . . . . .
H52 H 1.499(4) 1.260(4) 1.296(4) 0.137(18) Uiso 1 1 d . . . . .
H56 H 1.276(4) 1.317(4) 1.360(4) 0.132(16) Uiso 1 1 d . . . . .
H64 H 1.226(4) 0.742(4) 0.730(4) 0.151(19) Uiso 1 1 d . . . . .
H18 H -0.403(6) -0.198(5) -0.024(5) 0.19(3) Uiso 1 1 d . . . . .
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'
B B 0.0090 0.0039 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -3 -1 0.0414
0 -3 -1 0.0746
-2 3 1 0.0504
0 3 1 0.0744
3 -1 -3 0.0363
3 -2 0 0.0822
-3 2 0 0.0838
0 -3 2 0.0499
-2 0 3 0.0737
3 0 1 0.0960
-3 0 -1 0.0960
-1 3 -2 0.0357
-1 1 3 0.0662
0 3 -2 0.0280
1 0 -3 0.0491
1 -3 2 0.0477
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
C1 N1 C16 124.8(2) . . ?
C1 N1 C3 106.5(2) . . ?
C3 N1 C16 128.1(2) . . ?
C46 N4 C60 106.7(3) . . ?
C46 N4 B2 110.0(2) . . ?
C60 N4 B2 143.2(3) . . ?
C46 N3 C61 122.7(3) . . ?
C46 N3 C47 107.0(3) . . ?
C47 N3 C61 128.9(2) . . ?
C1 N2 C2 107.0(2) . . ?
C1 N2 B1 110.5(2) . . ?
C2 N2 B1 142.4(3) . . ?
C30 C31 C32 120.9(3) . . ?
C30 C31 C34 130.8(3) . . ?
C32 C31 C34 108.3(2) . . ?
C31 C30 C29 119.1(3) . . ?
C31 C30 H30 115.3(18) . . ?
C29 C30 H30 125.5(18) . . ?
N1 C1 C22 134.1(3) . . ?
N2 C1 N1 111.2(3) . . ?
N2 C1 C22 114.6(3) . . ?
C33 C28 C25 121.2(3) . . ?
C33 C28 C29 118.2(3) . . ?
C29 C28 C25 120.5(3) . . ?
C31 C32 C67 111.1(2) . . ?
C33 C32 C31 119.5(3) . . ?
C33 C32 C67 129.3(3) . . ?
C39 C34 C31 108.6(3) . . ?
C39 C34 C35 121.2(3) . . ?
C35 C34 C31 130.2(3) . . ?
C21 C16 N1 119.6(3) . . ?
C17 C16 N1 119.0(3) . . ?
C17 C16 C21 121.3(4) . . ?
C66 C61 N3 120.5(3) . . ?
C62 C61 N3 118.7(3) . . ?
C62 C61 C66 120.7(4) . . ?
C24 C25 C28 120.6(3) . . ?
C24 C25 C26 118.7(3) . . ?
C26 C25 C28 120.7(3) . . ?
C27 C22 C1 106.4(3) . . ?
C23 C22 C1 131.6(3) . . ?
C23 C22 C27 122.0(3) . . ?
N1 C3 C4 129.6(3) . . ?
C2 C3 N1 106.7(2) . . ?
C2 C3 C4 123.4(3) . . ?
C34 C39 C38 119.8(3) . . ?
C34 C39 C67 111.7(2) . . ?
C38 C39 C67 128.5(3) . . ?
C28 C33 H33 122(2) . . ?
C32 C33 C28 120.8(3) . . ?
C32 C33 H33 118(2) . . ?
C25 C24 H24 118(2) . . ?
C23 C24 C25 121.3(3) . . ?
C23 C24 H24 121(2) . . ?
C25 C26 H26 115(2) . . ?
C27 C26 C25 122.0(3) . . ?
C27 C26 H26 123(2) . . ?
N4 C46 N3 111.5(3) . . ?
N4 C46 C43 114.8(3) . . ?
N3 C46 C43 133.7(3) . . ?
C22 C27 B1 113.2(3) . . ?
C26 C27 C22 117.2(3) . . ?
C26 C27 B1 129.5(3) . . ?
N2 C2 C15 129.9(3) . . ?
C3 C2 N2 108.5(3) . . ?
C3 C2 C15 121.6(3) . . ?
C30 C29 C28 121.3(3) . . ?
C30 C29 H29 119.5(18) . . ?
C28 C29 H29 118.6(18) . . ?
C39 C38 C37 119.8(3) . . ?
C39 C38 H38 123(2) . . ?
C37 C38 H38 117(2) . . ?
N3 C47 C48 130.4(3) . . ?
C60 C47 N3 106.1(2) . . ?
C60 C47 C48 123.5(3) . . ?
C9 C4 C3 116.2(3) . . ?
C5 C4 C3 124.8(3) . . ?
C5 C4 C9 119.0(3) . . ?
C38 C37 C40 120.9(3) . . ?
C36 C37 C38 118.8(3) . . ?
C36 C37 C40 120.3(3) . . ?
N4 C60 C59 129.2(3) . . ?
C47 C60 N4 108.7(3) . . ?
C47 C60 C59 121.8(3) . . ?
C34 C35 H35 120.8(19) . . ?
C36 C35 C34 118.9(3) . . ?
C36 C35 H35 120.0(19) . . ?
C22 C23 H23 118(2) . . ?
C24 C23 C22 118.8(3) . . ?
C24 C23 H23 123(2) . . ?
C44 C45 H45 115.7(19) . . ?
C40 C45 C44 122.3(3) . . ?
C40 C45 H45 121.9(19) . . ?
C44 C43 C46 106.8(3) . . ?
C42 C43 C46 130.0(3) . . ?
C42 C43 C44 123.3(3) . . ?
C45 C44 C43 116.3(3) . . ?
C45 C44 B2 130.7(3) . . ?
C43 C44 B2 113.0(3) . . ?
C10 C15 C2 117.2(3) . . ?
C14 C15 C2 122.4(3) . . ?
C14 C15 C10 120.3(3) . . ?
C32 C67 C74 112.1(3) . . ?
C39 C67 C32 100.1(2) . . ?
C39 C67 C74 109.0(3) . . ?
C39 C67 C68 111.3(3) . . ?
C68 C67 C32 112.7(3) . . ?
C68 C67 C74 111.0(3) . . ?
C15 C10 C9 120.7(3) . . ?
C11 C10 C15 117.0(3) . . ?
C11 C10 C9 122.3(3) . . ?
C45 C40 C37 122.0(3) . . ?
C45 C40 C41 118.8(3) . . ?
C41 C40 C37 119.2(3) . . ?
C4 C9 C10 120.7(3) . . ?
C4 C9 C8 118.3(3) . . ?
C8 C9 C10 121.0(3) . . ?
C37 C36 H36 117(2) . . ?
C35 C36 C37 121.4(3) . . ?
C35 C36 H36 122(2) . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
B2 C82 H82A 109.5 . . ?
B2 C82 H82B 109.5 . . ?
B2 C82 H82C 109.5 . . ?
C54 C59 C60 116.4(3) . . ?
C58 C59 C60 124.1(3) . . ?
C58 C59 C54 119.4(3) . . ?
C4 C5 H5 121(2) . . ?
C6 C5 C4 120.6(4) . . ?
C6 C5 H5 118(2) . . ?
C53 C48 C47 115.3(3) . . ?
C49 C48 C47 124.7(3) . . ?
C49 C48 C53 120.0(3) . . ?
C61 C66 C65 119.2(4) . . ?
C61 C66 H66 115.3(19) . . ?
C65 C66 H66 125.5(19) . . ?
C16 C21 C20 118.1(5) . . ?
C16 C21 H21 117(2) . . ?
C20 C21 H21 125(2) . . ?
C67 C74 H74A 110(2) . . ?
C67 C74 H74B 111(2) . . ?
C75 C74 C67 117.2(3) . . ?
C75 C74 H74A 104(2) . . ?
C75 C74 H74B 102(2) . . ?
H74A C74 H74B 113(3) . . ?
C61 C62 C63 118.9(4) . . ?
C61 C62 H62 120(2) . . ?
C63 C62 H62 121(2) . . ?
C9 C8 H8 121(2) . . ?
C7 C8 C9 121.2(4) . . ?
C7 C8 H8 117.4(19) . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 H6 123(3) . . ?
C7 C6 H6 116(3) . . ?
C48 C53 C54 121.5(3) . . ?
C52 C53 C48 116.6(4) . . ?
C52 C53 C54 121.8(4) . . ?
C40 C41 H41 124(2) . . ?
C42 C41 C40 121.5(3) . . ?
C42 C41 H41 115(2) . . ?
C67 C68 H68A 110(2) . . ?
C67 C68 H68B 112(2) . . ?
C69 C68 C67 115.3(3) . . ?
C69 C68 H68A 110(2) . . ?
C69 C68 H68B 110(2) . . ?
H68A C68 H68B 99(3) . . ?
C43 C42 H42 124(2) . . ?
C41 C42 C43 117.8(3) . . ?
C41 C42 H42 118(2) . . ?
C59 C54 C53 120.6(3) . . ?
C55 C54 C59 117.2(4) . . ?
C55 C54 C53 122.2(4) . . ?
C15 C14 H14 122(3) . . ?
C13 C14 C15 120.4(4) . . ?
C13 C14 H14 117(3) . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 H7 120(3) . . ?
C6 C7 H7 120(3) . . ?
C59 C58 H58 116(3) . . ?
C57 C58 C59 121.8(5) . . ?
C57 C58 H58 122(3) . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
B2 C83 H83A 109.5 . . ?
B2 C83 H83B 109.5 . . ?
B2 C83 H83C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
B1 C80 H80A 109.5 . . ?
B1 C80 H80B 109.5 . . ?
B1 C80 H80C 109.5 . . ?
C10 C11 H11 119(2) . . ?
C12 C11 C10 121.7(4) . . ?
C12 C11 H11 119(2) . . ?
C16 C17 C18 119.5(5) . . ?
C16 C17 H17 122(4) . . ?
C18 C17 H17 119(4) . . ?
C48 C49 H49 125(3) . . ?
C50 C49 C48 121.4(5) . . ?
C50 C49 H49 113(3) . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
B1 C81 H81A 109.5 . . ?
B1 C81 H81B 109.5 . . ?
B1 C81 H81C 109.5 . . ?
C66 C65 H65 118(3) . . ?
C64 C65 C66 120.4(4) . . ?
C64 C65 H65 122(3) . . ?
C11 C12 C13 121.0(4) . . ?
C11 C12 H12 116(3) . . ?
C13 C12 H12 122(3) . . ?
C65 C64 H64 114(3) . . ?
C63 C64 C65 120.0(5) . . ?
C63 C64 H64 126(3) . . ?
C44 B2 N4 95.3(2) . . ?
C82 B2 N4 108.8(3) . . ?
C82 B2 C44 112.1(3) . . ?
C83 B2 N4 111.8(3) . . ?
C83 B2 C44 112.4(3) . . ?
C83 B2 C82 114.7(3) . . ?
C27 B1 N2 95.2(2) . . ?
C27 B1 C81 110.8(3) . . ?
C80 B1 N2 111.0(3) . . ?
C80 B1 C27 112.6(3) . . ?
C80 B1 C81 114.9(3) . . ?
C81 B1 N2 110.8(3) . . ?
C21 C20 H20 112(3) . . ?
C19 C20 C21 121.2(5) . . ?
C19 C20 H20 127(3) . . ?
C74 C75 H75A 108.6 . . ?
C74 C75 H75B 108.6 . . ?
H75A C75 H75B 107.5 . . ?
C76 C75 C74 114.9(4) . . ?
C76 C75 H75A 108.6 . . ?
C76 C75 H75B 108.6 . . ?
C49 C50 C51 119.0(5) . . ?
C49 C50 H50 116(3) . . ?
C51 C50 H50 125(3) . . ?
C62 C63 H63 114(3) . . ?
C64 C63 C62 120.9(5) . . ?
C64 C63 H63 125(3) . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 118(3) . . ?
C12 C13 H13 122(3) . . ?
C53 C52 H52 115(3) . . ?
C51 C52 C53 122.3(5) . . ?
C51 C52 H52 123(3) . . ?
C20 C19 C18 120.5(5) . . ?
C20 C19 H19 120(3) . . ?
C18 C19 H19 118(3) . . ?
C68 C69 H69A 108.2 . . ?
C68 C69 H69B 108.2 . . ?
C68 C69 C70 116.4(4) . . ?
H69A C69 H69B 107.4 . . ?
C70 C69 H69A 108.2 . . ?
C70 C69 H69B 108.2 . . ?
C17 C18 H18 124(5) . . ?
C19 C18 C17 119.3(6) . . ?
C19 C18 H18 117(5) . . ?
C58 C57 C56 118.8(5) . . ?
C58 C57 H57 118(3) . . ?
C56 C57 H57 123(3) . . ?
C54 C55 H55 118(3) . . ?
C56 C55 C54 121.7(5) . . ?
C56 C55 H55 120(3) . . ?
C50 C51 H51 118(3) . . ?
C52 C51 C50 120.7(4) . . ?
C52 C51 H51 121(3) . . ?
C57 C56 H56 120(3) . . ?
C55 C56 C57 121.0(5) . . ?
C55 C56 H56 117(3) . . ?
C75 C76 H76A 109.3 . . ?
C75 C76 H76B 109.3 . . ?
C75 C76 C77 111.4(5) . . ?
H76A C76 H76B 108.0 . . ?
C77 C76 H76A 109.3 . . ?
C77 C76 H76B 109.3 . . ?
C69 C70 H70A 108.4 . . ?
C69 C70 H70B 108.4 . . ?
H70A C70 H70B 107.5 . . ?
C71 C70 C69 115.4(5) . . ?
C71 C70 H70A 108.4 . . ?
C71 C70 H70B 108.4 . . ?
H72A C72 H72B 108.0 . . ?
C73 C72 H72A 109.4 . . ?
C73 C72 H72B 109.4 . . ?
C71 C72 H72A 109.4 . . ?
C71 C72 H72B 109.4 . . ?
C71 C72 C73 111.0(8) . . ?
C76 C77 H77A 108.8 . . ?
C76 C77 H77B 108.8 . . ?
H77A C77 H77B 107.7 . . ?
C78 C77 C76 113.7(8) . . ?
C78 C77 H77A 108.8 . . ?
C78 C77 H77B 108.8 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
C77 C78 C79 115.6(9) . . ?
C77 C78 H78A 108.4 . . ?
C77 C78 H78B 108.4 . . ?
C79 C78 H78A 108.4 . . ?
C79 C78 H78B 108.4 . . ?
H78A C78 H78B 107.4 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C70 C71 C72 119.0(6) . . ?
C70 C71 H71A 107.6 . . ?
C70 C71 H71B 107.6 . . ?
C72 C71 H71A 107.6 . . ?
C72 C71 H71B 107.6 . . ?
H71A C71 H71B 107.0 . . ?
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
N1 C1 1.356(4) . ?
N1 C16 1.447(4) . ?
N1 C3 1.402(4) . ?
N4 C46 1.329(4) . ?
N4 C60 1.387(4) . ?
N4 B2 1.654(4) . ?
N3 C61 1.437(4) . ?
N3 C46 1.348(4) . ?
N3 C47 1.405(4) . ?
N2 C1 1.325(4) . ?
N2 C2 1.389(4) . ?
N2 B1 1.653(4) . ?
C31 C30 1.384(4) . ?
C31 C32 1.391(4) . ?
C31 C34 1.471(4) . ?
C30 C29 1.384(4) . ?
C30 H30 0.99(3) . ?
C1 C22 1.451(4) . ?
C28 C25 1.489(4) . ?
C28 C33 1.401(4) . ?
C28 C29 1.403(4) . ?
C32 C33 1.383(4) . ?
C32 C67 1.535(4) . ?
C34 C39 1.379(4) . ?
C34 C35 1.388(4) . ?
C16 C21 1.371(5) . ?
C16 C17 1.356(5) . ?
C61 C66 1.371(5) . ?
C61 C62 1.367(5) . ?
C25 C24 1.392(4) . ?
C25 C26 1.396(4) . ?
C22 C27 1.409(4) . ?
C22 C23 1.390(4) . ?
C3 C2 1.368(4) . ?
C3 C4 1.443(4) . ?
C39 C38 1.394(4) . ?
C39 C67 1.529(4) . ?
C33 H33 0.95(3) . ?
C24 C23 1.382(4) . ?
C24 H24 0.99(4) . ?
C26 C27 1.388(4) . ?
C26 H26 1.00(4) . ?
C46 C43 1.450(4) . ?
C27 B1 1.606(5) . ?
C2 C15 1.432(4) . ?
C29 H29 1.06(3) . ?
C38 C37 1.402(5) . ?
C38 H38 1.00(4) . ?
C47 C60 1.377(4) . ?
C47 C48 1.424(4) . ?
C4 C9 1.410(5) . ?
C4 C5 1.404(5) . ?
C37 C40 1.488(4) . ?
C37 C36 1.395(5) . ?
C60 C59 1.427(5) . ?
C35 C36 1.378(4) . ?
C35 H35 1.08(4) . ?
C23 H23 0.88(3) . ?
C45 C44 1.398(4) . ?
C45 C40 1.382(5) . ?
C45 H45 1.00(3) . ?
C43 C44 1.400(4) . ?
C43 C42 1.390(5) . ?
C44 B2 1.611(5) . ?
C15 C10 1.418(4) . ?
C15 C14 1.395(5) . ?
C67 C74 1.545(4) . ?
C67 C68 1.530(4) . ?
C10 C9 1.473(5) . ?
C10 C11 1.402(5) . ?
C40 C41 1.398(5) . ?
C9 C8 1.411(5) . ?
C36 H36 1.07(4) . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
C82 B2 1.610(5) . ?
C59 C54 1.421(5) . ?
C59 C58 1.405(6) . ?
C5 C6 1.365(5) . ?
C5 H5 0.99(4) . ?
C48 C53 1.421(5) . ?
C48 C49 1.390(6) . ?
C66 C65 1.390(6) . ?
C66 H66 1.05(4) . ?
C21 C20 1.378(6) . ?
C21 H21 0.94(4) . ?
C74 C75 1.521(4) . ?
C74 H74A 1.00(3) . ?
C74 H74B 1.12(5) . ?
C62 C63 1.396(6) . ?
C62 H62 1.04(4) . ?
C8 C7 1.364(6) . ?
C8 H8 0.99(3) . ?
C6 C7 1.382(6) . ?
C6 H6 0.94(5) . ?
C53 C54 1.452(6) . ?
C53 C52 1.412(5) . ?
C41 C42 1.378(5) . ?
C41 H41 0.95(4) . ?
C68 C69 1.500(5) . ?
C68 H68A 1.03(4) . ?
C68 H68B 1.04(4) . ?
C42 H42 0.93(4) . ?
C54 C55 1.401(6) . ?
C14 C13 1.378(5) . ?
C14 H14 0.95(4) . ?
C7 H7 0.98(5) . ?
C58 C57 1.361(6) . ?
C58 H58 0.92(5) . ?
C83 H83A 0.9600 . ?
C83 H83B 0.9600 . ?
C83 H83C 0.9600 . ?
C83 B2 1.609(5) . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
C80 B1 1.604(6) . ?
C11 C12 1.362(6) . ?
C11 H11 0.94(4) . ?
C17 C18 1.396(7) . ?
C17 H17 0.95(6) . ?
C49 C50 1.372(5) . ?
C49 H49 0.85(4) . ?
C81 H81A 0.9600 . ?
C81 H81B 0.9600 . ?
C81 H81C 0.9600 . ?
C81 B1 1.610(5) . ?
C65 C64 1.368(7) . ?
C65 H65 1.04(5) . ?
C12 C13 1.380(6) . ?
C12 H12 0.96(5) . ?
C64 C63 1.346(7) . ?
C64 H64 1.07(6) . ?
C20 C19 1.354(8) . ?
C20 H20 0.90(5) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C75 C76 1.506(5) . ?
C50 C51 1.395(7) . ?
C50 H50 1.00(5) . ?
C63 H63 0.94(4) . ?
C13 H13 1.08(5) . ?
C52 C51 1.348(7) . ?
C52 H52 1.01(5) . ?
C19 C18 1.354(8) . ?
C19 H19 1.04(5) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C69 C70 1.507(5) . ?
C18 H18 0.87(7) . ?
C57 C56 1.390(7) . ?
C57 H57 1.08(6) . ?
C55 C56 1.369(8) . ?
C55 H55 1.04(6) . ?
C51 H51 0.99(5) . ?
C56 H56 1.02(5) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 C77 1.531(6) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C70 C71 1.482(6) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C72 C73 1.514(7) . ?
C72 C71 1.483(6) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C77 C78 1.433(7) . ?
C79 H79A 0.9600 . ?
C79 H79B 0.9600 . ?
C79 H79C 0.9600 . ?
C79 C78 1.518(7) . ?
C78 H78A 0.9700 . ?
C78 H78B 0.9700 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
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
N1 C1 C22 C27 -176.7(3) . . . . ?
N1 C1 C22 C23 1.7(6) . . . . ?
N1 C16 C21 C20 178.6(3) . . . . ?
N1 C16 C17 C18 -178.6(4) . . . . ?
N1 C3 C2 N2 -0.8(4) . . . . ?
N1 C3 C2 C15 179.3(3) . . . . ?
N1 C3 C4 C9 179.1(3) . . . . ?
N1 C3 C4 C5 1.8(6) . . . . ?
N4 C46 C43 C44 0.5(4) . . . . ?
N4 C46 C43 C42 -179.3(4) . . . . ?
N4 C60 C59 C54 -175.7(3) . . . . ?
N4 C60 C59 C58 1.8(6) . . . . ?
N3 C61 C66 C65 173.7(3) . . . . ?
N3 C61 C62 C63 -174.0(4) . . . . ?
N3 C46 C43 C44 178.6(4) . . . . ?
N3 C46 C43 C42 -1.1(7) . . . . ?
N3 C47 C60 N4 1.8(3) . . . . ?
N3 C47 C60 C59 -173.1(3) . . . . ?
N3 C47 C48 C53 175.5(3) . . . . ?
N3 C47 C48 C49 -7.4(6) . . . . ?
N2 C1 C22 C27 1.1(4) . . . . ?
N2 C1 C22 C23 179.5(4) . . . . ?
N2 C2 C15 C10 -178.0(3) . . . . ?
N2 C2 C15 C14 4.7(6) . . . . ?
C31 C30 C29 C28 0.3(5) . . . . ?
C31 C32 C33 C28 2.5(5) . . . . ?
C31 C32 C67 C39 2.9(3) . . . . ?
C31 C32 C67 C74 -112.5(3) . . . . ?
C31 C32 C67 C68 121.3(3) . . . . ?
C31 C34 C39 C38 -178.8(3) . . . . ?
C31 C34 C39 C67 0.0(4) . . . . ?
C31 C34 C35 C36 177.9(3) . . . . ?
C30 C31 C32 C33 -4.1(5) . . . . ?
C30 C31 C32 C67 177.5(3) . . . . ?
C30 C31 C34 C39 -178.8(3) . . . . ?
C30 C31 C34 C35 2.3(6) . . . . ?
C1 N1 C16 C21 83.9(4) . . . . ?
C1 N1 C16 C17 -97.5(4) . . . . ?
C1 N1 C3 C2 1.0(3) . . . . ?
C1 N1 C3 C4 -172.6(3) . . . . ?
C1 N2 C2 C3 0.3(4) . . . . ?
C1 N2 C2 C15 -179.8(3) . . . . ?
C1 N2 B1 C27 -0.2(3) . . . . ?
C1 N2 B1 C80 -116.8(3) . . . . ?
C1 N2 B1 C81 114.3(3) . . . . ?
C1 C22 C27 C26 177.9(3) . . . . ?
C1 C22 C27 B1 -1.2(4) . . . . ?
C1 C22 C23 C24 -177.8(3) . . . . ?
C28 C25 C24 C23 179.8(3) . . . . ?
C28 C25 C26 C27 179.9(3) . . . . ?
C32 C31 C30 C29 2.7(5) . . . . ?
C32 C31 C34 C39 2.0(4) . . . . ?
C32 C31 C34 C35 -176.9(4) . . . . ?
C32 C67 C74 C75 -63.1(5) . . . . ?
C32 C67 C68 C69 -54.2(4) . . . . ?
C34 C31 C30 C29 -176.5(3) . . . . ?
C34 C31 C32 C33 175.2(3) . . . . ?
C34 C31 C32 C67 -3.2(4) . . . . ?
C34 C39 C38 C37 0.4(5) . . . . ?
C34 C39 C67 C32 -1.7(4) . . . . ?
C34 C39 C67 C74 116.0(3) . . . . ?
C34 C39 C67 C68 -121.1(3) . . . . ?
C34 C35 C36 C37 1.0(6) . . . . ?
C16 N1 C1 N2 171.1(3) . . . . ?
C16 N1 C1 C22 -11.1(6) . . . . ?
C16 N1 C3 C2 -170.5(3) . . . . ?
C16 N1 C3 C4 15.9(5) . . . . ?
C16 C21 C20 C19 -1.4(7) . . . . ?
C16 C17 C18 C19 1.3(8) . . . . ?
C61 N3 C46 N4 -167.5(3) . . . . ?
C61 N3 C46 C43 14.3(5) . . . . ?
C61 N3 C47 C60 165.2(3) . . . . ?
C61 N3 C47 C48 -16.9(5) . . . . ?
C61 C66 C65 C64 1.0(6) . . . . ?
C61 C62 C63 C64 -0.6(7) . . . . ?
C25 C28 C33 C32 178.6(3) . . . . ?
C25 C28 C29 C30 180.0(3) . . . . ?
C25 C24 C23 C22 -0.1(6) . . . . ?
C25 C26 C27 C22 0.7(5) . . . . ?
C25 C26 C27 B1 179.6(3) . . . . ?
C22 C27 B1 N2 0.9(3) . . . . ?
C22 C27 B1 C80 116.2(3) . . . . ?
C22 C27 B1 C81 -113.7(3) . . . . ?
C3 N1 C1 N2 -0.8(4) . . . . ?
C3 N1 C1 C22 177.1(3) . . . . ?
C3 N1 C16 C21 -106.1(4) . . . . ?
C3 N1 C16 C17 72.6(4) . . . . ?
C3 C2 C15 C10 1.9(5) . . . . ?
C3 C2 C15 C14 -175.4(3) . . . . ?
C3 C4 C9 C10 -1.9(5) . . . . ?
C3 C4 C9 C8 179.9(3) . . . . ?
C3 C4 C5 C6 177.8(3) . . . . ?
C39 C34 C35 C36 -0.9(5) . . . . ?
C39 C38 C37 C40 178.6(3) . . . . ?
C39 C38 C37 C36 -0.4(5) . . . . ?
C39 C67 C74 C75 -173.0(3) . . . . ?
C39 C67 C68 C69 57.4(4) . . . . ?
C33 C28 C25 C24 150.7(3) . . . . ?
C33 C28 C25 C26 -29.7(5) . . . . ?
C33 C28 C29 C30 -1.9(5) . . . . ?
C33 C32 C67 C39 -175.2(3) . . . . ?
C33 C32 C67 C74 69.3(4) . . . . ?
C33 C32 C67 C68 -56.8(5) . . . . ?
C24 C25 C26 C27 -0.4(5) . . . . ?
C26 C25 C24 C23 0.1(5) . . . . ?
C26 C27 B1 N2 -178.1(3) . . . . ?
C26 C27 B1 C80 -62.8(5) . . . . ?
C26 C27 B1 C81 67.4(5) . . . . ?
C46 N4 C60 C47 -2.0(3) . . . . ?
C46 N4 C60 C59 172.4(3) . . . . ?
C46 N4 B2 C44 -1.5(3) . . . . ?
C46 N4 B2 C82 114.1(3) . . . . ?
C46 N4 B2 C83 -118.2(3) . . . . ?
C46 N3 C61 C66 -99.4(4) . . . . ?
C46 N3 C61 C62 75.8(4) . . . . ?
C46 N3 C47 C60 -0.9(3) . . . . ?
C46 N3 C47 C48 177.0(3) . . . . ?
C46 C43 C44 C45 178.2(3) . . . . ?
C46 C43 C44 B2 -1.6(4) . . . . ?
C46 C43 C42 C41 -178.8(4) . . . . ?
C27 C22 C23 C24 0.4(5) . . . . ?
C2 N2 C1 N1 0.3(4) . . . . ?
C2 N2 C1 C22 -178.0(3) . . . . ?
C2 N2 B1 C27 175.9(4) . . . . ?
C2 N2 B1 C80 59.3(5) . . . . ?
C2 N2 B1 C81 -69.5(5) . . . . ?
C2 C3 C4 C9 6.4(5) . . . . ?
C2 C3 C4 C5 -170.8(3) . . . . ?
C2 C15 C10 C9 2.5(5) . . . . ?
C2 C15 C10 C11 -178.7(3) . . . . ?
C2 C15 C14 C13 176.9(4) . . . . ?
C29 C28 C25 C24 -31.2(5) . . . . ?
C29 C28 C25 C26 148.4(3) . . . . ?
C29 C28 C33 C32 0.4(5) . . . . ?
C38 C39 C67 C32 177.0(3) . . . . ?
C38 C39 C67 C74 -65.3(4) . . . . ?
C38 C39 C67 C68 57.6(4) . . . . ?
C38 C37 C40 C45 36.8(5) . . . . ?
C38 C37 C40 C41 -143.0(4) . . . . ?
C38 C37 C36 C35 -0.3(6) . . . . ?
C47 N3 C61 C66 96.4(4) . . . . ?
C47 N3 C61 C62 -88.4(4) . . . . ?
C47 N3 C46 N4 -0.3(4) . . . . ?
C47 N3 C46 C43 -178.5(3) . . . . ?
C47 C60 C59 C54 -2.0(5) . . . . ?
C47 C60 C59 C58 175.5(4) . . . . ?
C47 C48 C53 C54 -1.2(5) . . . . ?
C47 C48 C53 C52 176.9(3) . . . . ?
C47 C48 C49 C50 -176.1(4) . . . . ?
C4 C3 C2 N2 173.3(3) . . . . ?
C4 C3 C2 C15 -6.6(5) . . . . ?
C4 C9 C8 C7 2.4(6) . . . . ?
C4 C5 C6 C7 2.0(6) . . . . ?
C37 C40 C41 C42 177.8(4) . . . . ?
C60 N4 C46 N3 1.4(4) . . . . ?
C60 N4 C46 C43 180.0(3) . . . . ?
C60 N4 B2 C44 179.8(4) . . . . ?
C60 N4 B2 C82 -64.7(5) . . . . ?
C60 N4 B2 C83 63.0(5) . . . . ?
C60 C47 C48 C53 -7.0(5) . . . . ?
C60 C47 C48 C49 170.1(4) . . . . ?
C60 C59 C54 C53 -5.9(5) . . . . ?
C60 C59 C54 C55 174.7(4) . . . . ?
C60 C59 C58 C57 -175.0(4) . . . . ?
C35 C34 C39 C38 0.2(5) . . . . ?
C35 C34 C39 C67 179.0(3) . . . . ?
C23 C22 C27 C26 -0.7(5) . . . . ?
C23 C22 C27 B1 -179.8(3) . . . . ?
C45 C44 B2 N4 -178.0(3) . . . . ?
C45 C44 B2 C82 69.3(4) . . . . ?
C45 C44 B2 C83 -61.7(5) . . . . ?
C45 C40 C41 C42 -1.9(6) . . . . ?
C43 C44 B2 N4 1.8(3) . . . . ?
C43 C44 B2 C82 -110.9(3) . . . . ?
C43 C44 B2 C83 118.0(3) . . . . ?
C44 C45 C40 C37 -178.4(3) . . . . ?
C44 C45 C40 C41 1.3(6) . . . . ?
C44 C43 C42 C41 1.5(6) . . . . ?
C15 C10 C9 C4 -2.4(5) . . . . ?
C15 C10 C9 C8 175.8(3) . . . . ?
C15 C10 C11 C12 2.2(6) . . . . ?
C15 C14 C13 C12 1.3(7) . . . . ?
C67 C32 C33 C28 -179.5(3) . . . . ?
C67 C39 C38 C37 -178.1(3) . . . . ?
C67 C74 C75 C76 -176.4(4) . . . . ?
C67 C68 C69 C70 177.2(4) . . . . ?
C10 C15 C14 C13 -0.3(6) . . . . ?
C10 C9 C8 C7 -175.9(4) . . . . ?
C10 C11 C12 C13 -1.3(7) . . . . ?
C40 C37 C36 C35 -179.3(3) . . . . ?
C40 C45 C44 C43 0.5(5) . . . . ?
C40 C45 C44 B2 -179.7(3) . . . . ?
C40 C41 C42 C43 0.5(6) . . . . ?
C9 C4 C5 C6 0.6(5) . . . . ?
C9 C10 C11 C12 -179.0(4) . . . . ?
C9 C8 C7 C6 0.2(6) . . . . ?
C36 C37 C40 C45 -144.3(4) . . . . ?
C36 C37 C40 C41 36.0(5) . . . . ?
C59 C54 C55 C56 0.9(8) . . . . ?
C59 C58 C57 C56 0.0(8) . . . . ?
C5 C4 C9 C10 175.5(3) . . . . ?
C5 C4 C9 C8 -2.7(5) . . . . ?
C5 C6 C7 C8 -2.4(7) . . . . ?
C48 C47 C60 N4 -176.3(3) . . . . ?
C48 C47 C60 C59 8.9(5) . . . . ?
C48 C53 C54 C59 7.7(6) . . . . ?
C48 C53 C54 C55 -173.0(4) . . . . ?
C48 C53 C52 C51 -0.4(7) . . . . ?
C48 C49 C50 C51 -0.7(8) . . . . ?
C66 C61 C62 C63 1.2(6) . . . . ?
C66 C65 C64 C63 -0.4(7) . . . . ?
C21 C16 C17 C18 0.0(6) . . . . ?
C21 C20 C19 C18 2.8(8) . . . . ?
C74 C67 C68 C69 179.1(3) . . . . ?
C74 C75 C76 C77 172.6(6) . . . . ?
C62 C61 C66 C65 -1.4(5) . . . . ?
C53 C48 C49 C50 0.9(7) . . . . ?
C53 C54 C55 C56 -178.4(5) . . . . ?
C53 C52 C51 C50 0.6(9) . . . . ?
C68 C67 C74 C75 63.9(4) . . . . ?
C68 C69 C70 C71 -55.2(7) . . . . ?
C42 C43 C44 C45 -2.0(5) . . . . ?
C42 C43 C44 B2 178.2(3) . . . . ?
C54 C59 C58 C57 2.5(7) . . . . ?
C54 C53 C52 C51 177.7(5) . . . . ?
C54 C55 C56 C57 1.6(10) . . . . ?
C14 C15 C10 C9 179.8(3) . . . . ?
C14 C15 C10 C11 -1.4(5) . . . . ?
C58 C59 C54 C53 176.5(4) . . . . ?
C58 C59 C54 C55 -2.9(6) . . . . ?
C58 C57 C56 C55 -2.0(10) . . . . ?
C11 C10 C9 C4 178.8(3) . . . . ?
C11 C10 C9 C8 -2.9(5) . . . . ?
C11 C12 C13 C14 -0.5(8) . . . . ?
C17 C16 C21 C20 0.0(6) . . . . ?
C49 C48 C53 C54 -178.5(4) . . . . ?
C49 C48 C53 C52 -0.3(6) . . . . ?
C49 C50 C51 C52 0.0(9) . . . . ?
C65 C64 C63 C62 0.2(8) . . . . ?
B2 N4 C46 N3 -177.8(3) . . . . ?
B2 N4 C46 C43 0.8(4) . . . . ?
B2 N4 C60 C47 176.8(4) . . . . ?
B2 N4 C60 C59 -8.9(6) . . . . ?
B1 N2 C1 N1 177.8(3) . . . . ?
B1 N2 C1 C22 -0.5(4) . . . . ?
B1 N2 C2 C3 -175.9(4) . . . . ?
B1 N2 C2 C15 4.0(7) . . . . ?
C20 C19 C18 C17 -2.7(8) . . . . ?
C75 C76 C77 C78 97.0(11) . . . . ?
C52 C53 C54 C59 -170.4(4) . . . . ?
C52 C53 C54 C55 8.9(7) . . . . ?
C69 C70 C71 C72 -48.4(9) . . . . ?
C76 C77 C78 C79 176.2(10) . . . . ?
C73 C72 C71 C70 179.9(8) . . . . ?
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
1.9990 -2.9979 -1.0001 0.0312 -0.0281 0.3278
0.0013 -2.9945 -1.0047 -0.1101 -0.2229 0.2866
-1.9990 2.9979 1.0001 -0.0312 0.0281 -0.3278
-0.0013 2.9945 1.0047 0.1101 0.2229 -0.2866
2.9970 -0.9950 -2.9960 0.2634 -0.0553 0.2246
2.9974 -2.0036 0.0042 0.1164 0.2119 0.2361
-2.9974 2.0036 -0.0042 -0.1164 -0.2119 -0.2361
0.0013 -3.0039 1.9968 -0.2093 0.0845 0.2110
-1.9977 -0.0059 2.9969 -0.2405 0.1126 -0.1169
2.9965 -0.0083 1.0075 0.1787 0.3946 0.0366
-2.9965 0.0083 -1.0075 -0.1787 -0.3946 -0.0366
-1.0001 3.0056 -1.9992 0.1387 -0.1818 -0.2316
-0.9993 0.9916 3.0007 -0.1222 0.2501 -0.1834
-0.0013 3.0039 -1.9968 0.2093 -0.0845 -0.2110
0.9989 0.0076 -2.9993 0.1699 -0.2099 0.0962
1.0001 -3.0056 1.9992 -0.1387 0.1818 0.2316
