#------------------------------------------------------------------------------
#$Date: 2020-10-06 09:58:36 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257282 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557761.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_1557761
loop_
_publ_author_name
'Dong, Zhaowen'
'Pezzato, Cristian'
'Sienkiewicz, Andrzej'
'Scopelliti, Rosario'
'Fadaei-Tirani, Farzaneh'
'Severin, Kay'
_publ_section_title
;
 SET processes in Lewis acid--base reactions: the tritylation of
 N-heterocyclic carbenes
;
_journal_issue                   29
_journal_name_full               'Chemical Science'
_journal_page_first              7615
_journal_page_last               7618
_journal_paper_doi               10.1039/D0SC01278E
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C46 H51 N2, C24 B F20, C H2 Cl2'
_chemical_formula_sum            'C71 H53 B Cl2 F20 N2'
_chemical_formula_weight         1395.86
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-08
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_audit_update_record
;
2020-01-28 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                94.923(3)
_cell_angle_beta                 102.959(3)
_cell_angle_gamma                114.918(4)
_cell_formula_units_Z            2
_cell_length_a                   13.2446(5)
_cell_length_b                   13.7731(5)
_cell_length_c                   20.2266(8)
_cell_measurement_reflns_used    8509
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5760
_cell_measurement_theta_min      3.6280
_cell_volume                     3192.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.62a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.62a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.62a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -46.00 -10.00   1.00   10.00    --  -40.85 125.00   0.00   36
  2  ω   -118.00  -4.00   1.00   10.00    --  -40.85 -19.00 -90.00  114
  3  ω   -115.00 -22.00   1.00   10.00    --  -40.85 -38.00-150.00   93
  4  ω     28.00  92.00   1.00   10.00    --   40.85-125.00-180.00   64
  5  ω     28.00  53.00   1.00   10.00    --   40.85-125.00-150.00   25
  6  ω     51.00  93.00   1.00   10.00    --   40.85-128.00  49.00   42
  7  ω     34.00 133.00   1.00   40.00    --  105.15 -30.00-120.00   99
  8  ω     56.00  96.00   1.00   40.00    --  105.15-111.00 -60.00   40
  9  ω     98.00 125.00   1.00   40.00    --  105.15 -30.00  60.00   27
 10  ω     41.00 131.00   1.00   40.00    --  105.15 -30.00 -30.00   90
 11  ω    112.00 159.00   1.00   40.00    --  105.15  45.00 -90.00   47
 12  ω     31.00 104.00   1.00   40.00    --  105.15 -94.00 120.00   73
 13  ω     57.00 106.00   1.00   40.00    --  105.15-111.00  90.00   49
 14  ω    113.00 162.00   1.00   40.00    --  105.15  77.00 -60.00   49
 15  ω     83.00 109.00   1.00   40.00    --  105.15-111.00   0.00   26
 16  ω     61.00 109.00   1.00   40.00    --  105.15-111.00-120.00   48
 17  ω    115.00 147.00   1.00   40.00    --  105.15  77.00   0.00   32
 18  ω     40.00 121.00   1.00   40.00    --  105.15 -45.00 120.00   81
 19  ω    117.00 178.00   1.00   40.00    --  105.15  77.00  30.00   61
 20  ω     47.00  80.00   1.00   40.00    --  105.15 -30.00  60.00   33
 21  ω     48.00 119.00   1.00   40.00    --  105.15 -77.00 -60.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1245148000
_diffrn_orient_matrix_UB_12      0.0842402000
_diffrn_orient_matrix_UB_13      0.0047002000
_diffrn_orient_matrix_UB_21      0.0335407000
_diffrn_orient_matrix_UB_22      0.0152984000
_diffrn_orient_matrix_UB_23      0.0795546000
_diffrn_orient_matrix_UB_31      0.0362007000
_diffrn_orient_matrix_UB_32      -0.0924190000
_diffrn_orient_matrix_UB_33      -0.0047485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22810
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.742
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.62a (Rigaku Oxford Diffraction, 2019)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         12281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0433
_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)+(0.0578P)²+1.0365P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10158
_reflns_number_total             12281
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc01278e2.cif
_cod_data_source_block           dzw-112
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1557761--1557764.cif.

 Adding full bibliography for 1557761--1557764.cif.
;
_cod_original_cell_volume        3192.5(2)
_cod_database_code               1557761
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C71 H54 B Cl2 F20 N2'
_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.
;
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.600
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C4(H4), C29(H29), C32(H32), C41(H41), C44(H44)
2.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C37(H37), C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C)
;
_olex2_date_sample_data_collection 2019-11-07
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.844
_oxdiff_exptl_absorpt_empirical_full_min 0.696
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
Cl1 Cl -0.03193(6) 0.14518(6) 0.41229(4) 0.06164(18) Uani 1 1 d . . . . .
Cl2 Cl 0.08821(6) 0.01252(5) 0.39637(4) 0.05680(17) Uani 1 1 d . . . . .
C71 C 0.0194(3) 0.0849(3) 0.35675(17) 0.0661(8) Uani 1 1 d . . . . .
H71A H -0.046871 0.034479 0.316657 0.079 Uiso 1 1 calc R U . . .
H71B H 0.074719 0.142774 0.338873 0.079 Uiso 1 1 calc R U . . .
F1 F 0.80251(11) 0.42801(10) 0.26438(6) 0.0368(3) Uani 1 1 d . . . . .
F2 F 0.93608(15) 0.53150(13) 0.39283(8) 0.0572(4) Uani 1 1 d . . . . .
F3 F 1.12867(14) 0.50496(12) 0.44885(7) 0.0538(4) Uani 1 1 d . . . . .
F4 F 1.18656(10) 0.37688(10) 0.37050(7) 0.0400(3) Uani 1 1 d . . . . .
F5 F 1.05828(9) 0.27548(9) 0.24324(6) 0.0325(2) Uani 1 1 d . . . . .
F6 F 0.66851(10) 0.38500(9) 0.11371(6) 0.0333(2) Uani 1 1 d . . . . .
F7 F 0.72554(12) 0.55233(11) 0.05133(8) 0.0442(3) Uani 1 1 d . . . . .
F8 F 0.93722(12) 0.64573(10) 0.02698(7) 0.0422(3) Uani 1 1 d . . . . .
F9 F 1.09501(10) 0.57026(9) 0.07307(6) 0.0366(3) Uani 1 1 d . . . . .
F10 F 1.03834(9) 0.39877(8) 0.13389(6) 0.0290(2) Uani 1 1 d . . . . .
F11 F 0.84132(10) 0.10767(9) 0.23335(6) 0.0310(2) Uani 1 1 d . . . . .
F12 F 0.86182(12) -0.06521(10) 0.18231(7) 0.0403(3) Uani 1 1 d . . . . .
F13 F 0.88330(13) -0.09140(10) 0.05146(7) 0.0430(3) Uani 1 1 d . . . . .
F14 F 0.87701(11) 0.05751(10) -0.02701(6) 0.0366(3) Uani 1 1 d . . . . .
F15 F 0.85539(10) 0.22985(8) 0.02211(6) 0.0296(2) Uani 1 1 d . . . . .
F16 F 0.71930(11) 0.20830(9) 0.28762(6) 0.0355(3) Uani 1 1 d . . . . .
F17 F 0.50126(13) 0.06770(12) 0.27099(9) 0.0520(4) Uani 1 1 d . . . . .
F18 F 0.34611(11) -0.01928(11) 0.14174(10) 0.0576(4) Uani 1 1 d . . . . .
F19 F 0.41711(11) 0.04268(10) 0.02939(8) 0.0475(3) Uani 1 1 d . . . . .
F20 F 0.63626(10) 0.18479(9) 0.04470(6) 0.0342(3) Uani 1 1 d . . . . .
C47 C 0.91807(15) 0.34122(14) 0.24699(10) 0.0250(4) Uani 1 1 d . . . . .
C48 C 0.89720(17) 0.41209(15) 0.28869(11) 0.0303(4) Uani 1 1 d . . . . .
C49 C 0.9649(2) 0.46737(17) 0.35520(12) 0.0385(5) Uani 1 1 d . . . . .
C50 C 1.06272(19) 0.45469(17) 0.38370(11) 0.0373(5) Uani 1 1 d . . . . .
C51 C 1.09053(17) 0.38933(16) 0.34378(11) 0.0315(4) Uani 1 1 d . . . . .
C52 C 1.02035(16) 0.33578(15) 0.27744(10) 0.0269(4) Uani 1 1 d . . . . .
C53 C 0.84980(15) 0.37989(14) 0.12612(9) 0.0237(3) Uani 1 1 d . . . . .
C54 C 0.77583(16) 0.42573(15) 0.10442(10) 0.0258(4) Uani 1 1 d . . . . .
C55 C 0.80361(18) 0.51404(15) 0.07177(11) 0.0304(4) Uani 1 1 d . . . . .
C56 C 0.91053(18) 0.56294(15) 0.06058(10) 0.0301(4) Uani 1 1 d . . . . .
C57 C 0.98930(16) 0.52333(14) 0.08307(10) 0.0271(4) Uani 1 1 d . . . . .
C58 C 0.95750(15) 0.43486(14) 0.11437(9) 0.0240(3) Uani 1 1 d . . . . .
C59 C 0.85072(14) 0.18071(13) 0.13178(9) 0.0227(3) Uani 1 1 d . . . . .
C60 C 0.85088(15) 0.09926(14) 0.16846(10) 0.0251(4) Uani 1 1 d . . . . .
C61 C 0.86062(17) 0.00862(15) 0.14271(10) 0.0287(4) Uani 1 1 d . . . . .
C62 C 0.86996(17) -0.00551(15) 0.07683(10) 0.0298(4) Uani 1 1 d . . . . .
C63 C 0.86716(16) 0.07031(15) 0.03735(9) 0.0273(4) Uani 1 1 d . . . . .
C64 C 0.85725(15) 0.16065(14) 0.06507(10) 0.0245(3) Uani 1 1 d . . . . .
C65 C 0.69050(16) 0.20763(14) 0.16677(10) 0.0268(4) Uani 1 1 d . . . . .
C66 C 0.64896(17) 0.17324(15) 0.22214(11) 0.0304(4) Uani 1 1 d . . . . .
C67 C 0.53434(19) 0.09821(17) 0.21487(13) 0.0377(5) Uani 1 1 d . . . . .
C68 C 0.45649(17) 0.05384(16) 0.14996(14) 0.0401(5) Uani 1 1 d . . . . .
C69 C 0.49250(17) 0.08448(16) 0.09307(13) 0.0358(5) Uani 1 1 d . . . . .
C70 C 0.60668(16) 0.15959(15) 0.10277(11) 0.0290(4) Uani 1 1 d . . . . .
B1 B 0.82793(17) 0.27914(16) 0.16822(11) 0.0235(4) Uani 1 1 d . . . . .
N1 N 0.52719(12) 0.58541(11) 0.75269(8) 0.0208(3) Uani 1 1 d . . . . .
N2 N 0.44317(13) 0.41334(11) 0.75286(8) 0.0239(3) Uani 1 1 d . . . . .
C1 C 0.53149(15) 0.49084(13) 0.73661(9) 0.0213(3) Uani 1 1 d . . . . .
C2 C 0.43470(15) 0.56742(14) 0.77885(10) 0.0262(4) Uani 1 1 d . . . . .
H2 H 0.412356 0.620704 0.793799 0.031 Uiso 1 1 calc R U . . .
C3 C 0.38208(16) 0.45994(15) 0.77918(11) 0.0295(4) Uani 1 1 d . . . . .
H3 H 0.315634 0.422987 0.794542 0.035 Uiso 1 1 calc R U . . .
C4 C 0.62407(15) 0.48226(14) 0.70781(10) 0.0239(3) Uani 1 1 d . . . . .
H4 H 0.666960 0.554720 0.695984 0.029 Uiso 1 1 calc R U . . .
C5 C 0.71241(15) 0.46704(14) 0.76107(10) 0.0259(4) Uani 1 1 d . . . . .
H5 H 0.742925 0.511800 0.806130 0.031 Uiso 1 1 calc R U . . .
C6 C 0.75007(16) 0.39353(14) 0.74805(10) 0.0261(4) Uani 1 1 d . . . . .
H6 H 0.808305 0.390466 0.783815 0.031 Uiso 1 1 calc R U . . .
C7 C 0.70623(16) 0.31741(14) 0.68150(10) 0.0251(4) Uani 1 1 d . . . . .
C8 C 0.61629(16) 0.32667(14) 0.62976(10) 0.0262(4) Uani 1 1 d . . . . .
H8 H 0.584681 0.279162 0.585592 0.031 Uiso 1 1 calc R U . . .
C9 C 0.57608(16) 0.39882(15) 0.64141(10) 0.0264(4) Uani 1 1 d . . . . .
H9 H 0.514243 0.397319 0.606082 0.032 Uiso 1 1 calc R U . . .
C10 C 0.74688(17) 0.24405(15) 0.66903(10) 0.0278(4) Uani 1 1 d . . . . .
C11 C 0.82985(17) 0.22717(15) 0.72402(10) 0.0280(4) Uani 1 1 d . . . . .
C12 C 0.93345(19) 0.23359(18) 0.71413(11) 0.0367(4) Uani 1 1 d . . . . .
H12 H 0.950742 0.248500 0.671897 0.044 Uiso 1 1 calc R U . . .
C13 C 1.0111(2) 0.2184(2) 0.76550(12) 0.0411(5) Uani 1 1 d . . . . .
H13 H 1.081356 0.222993 0.758295 0.049 Uiso 1 1 calc R U . . .
C14 C 0.98701(19) 0.19653(17) 0.82700(11) 0.0363(4) Uani 1 1 d . . . . .
H14 H 1.041175 0.187672 0.862488 0.044 Uiso 1 1 calc R U . . .
C15 C 0.88348(19) 0.18757(16) 0.83684(11) 0.0339(4) Uani 1 1 d . . . . .
H15 H 0.865917 0.171202 0.878799 0.041 Uiso 1 1 calc R U . . .
C16 C 0.80554(17) 0.20246(15) 0.78552(11) 0.0305(4) Uani 1 1 d . . . . .
H16 H 0.734472 0.195661 0.792522 0.037 Uiso 1 1 calc R U . . .
C17 C 0.71244(19) 0.17362(17) 0.59967(11) 0.0329(4) Uani 1 1 d . . . . .
C18 C 0.6569(3) 0.06031(19) 0.59202(13) 0.0494(6) Uani 1 1 d . . . . .
H18 H 0.639131 0.029240 0.630604 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6273(3) -0.0074(2) 0.52923(15) 0.0673(9) Uani 1 1 d . . . . .
H19 H 0.588029 -0.084431 0.524846 0.081 Uiso 1 1 calc R U . . .
C20 C 0.6540(3) 0.0352(3) 0.47311(14) 0.0646(9) Uani 1 1 d . . . . .
H20 H 0.633162 -0.011880 0.429961 0.077 Uiso 1 1 calc R U . . .
C21 C 0.7114(3) 0.1473(3) 0.47992(14) 0.0620(8) Uani 1 1 d . . . . .
H21 H 0.731880 0.177508 0.441599 0.074 Uiso 1 1 calc R U . . .
C22 C 0.7393(2) 0.2162(2) 0.54285(13) 0.0471(6) Uani 1 1 d . . . . .
H22 H 0.777214 0.293224 0.546759 0.057 Uiso 1 1 calc R U . . .
C23 C 0.60554(15) 0.69188(13) 0.74421(9) 0.0223(3) Uani 1 1 d . . . . .
C24 C 0.58425(17) 0.71878(15) 0.67941(10) 0.0277(4) Uani 1 1 d . . . . .
C25 C 0.6592(2) 0.82368(16) 0.67409(12) 0.0359(4) Uani 1 1 d . . . . .
H25 H 0.649777 0.845045 0.630593 0.043 Uiso 1 1 calc R U . . .
C26 C 0.7469(2) 0.89680(16) 0.73106(12) 0.0387(5) Uani 1 1 d . . . . .
H26 H 0.795078 0.968585 0.726584 0.046 Uiso 1 1 calc R U . . .
C27 C 0.76551(18) 0.86712(15) 0.79435(11) 0.0337(4) Uani 1 1 d . . . . .
H27 H 0.826670 0.918607 0.832797 0.040 Uiso 1 1 calc R U . . .
C28 C 0.69574(16) 0.76242(14) 0.80281(10) 0.0257(4) Uani 1 1 d . . . . .
C29 C 0.48340(19) 0.63950(16) 0.61816(10) 0.0339(4) Uani 1 1 d . . . . .
H29 H 0.457696 0.564703 0.628874 0.041 Uiso 1 1 calc R U . . .
C30 C 0.5174(3) 0.6364(2) 0.55200(14) 0.0623(8) Uani 1 1 d . . . . .
H30A H 0.536074 0.706711 0.537674 0.093 Uiso 1 1 calc R U . . .
H30B H 0.452699 0.577823 0.515607 0.093 Uiso 1 1 calc R U . . .
H30C H 0.585636 0.622816 0.559707 0.093 Uiso 1 1 calc R U . . .
C31 C 0.3814(3) 0.6659(3) 0.60963(17) 0.0750(11) Uani 1 1 d . . . . .
H31A H 0.316010 0.612534 0.571099 0.113 Uiso 1 1 calc R U . . .
H31B H 0.404345 0.739483 0.599894 0.113 Uiso 1 1 calc R U . . .
H31C H 0.358119 0.662651 0.652399 0.113 Uiso 1 1 calc R U . . .
C32 C 0.71695(16) 0.72761(15) 0.87139(10) 0.0283(4) Uani 1 1 d . . . . .
H32 H 0.679078 0.645866 0.861986 0.034 Uiso 1 1 calc R U . . .
C33 C 0.84643(19) 0.76843(18) 0.90600(12) 0.0381(5) Uani 1 1 d . . . . .
H33A H 0.881317 0.746925 0.873196 0.057 Uiso 1 1 calc R U . . .
H33B H 0.856735 0.736273 0.946840 0.057 Uiso 1 1 calc R U . . .
H33C H 0.884405 0.848305 0.920176 0.057 Uiso 1 1 calc R U . . .
C34 C 0.66148(18) 0.76600(18) 0.92011(11) 0.0361(4) Uani 1 1 d . . . . .
H34A H 0.695352 0.845980 0.929043 0.054 Uiso 1 1 calc R U . . .
H34B H 0.676191 0.742018 0.963955 0.054 Uiso 1 1 calc R U . . .
H34C H 0.577458 0.734533 0.898472 0.054 Uiso 1 1 calc R U . . .
C35 C 0.40634(16) 0.29603(14) 0.73898(10) 0.0268(4) Uani 1 1 d . . . . .
C36 C 0.32819(17) 0.23637(15) 0.67445(11) 0.0296(4) Uani 1 1 d . . . . .
C37 C 0.29201(19) 0.12393(16) 0.66214(12) 0.0363(5) Uani 1 1 d . . . . .
H37 H 0.239014 0.079639 0.618883 0.044 Uiso 1 1 calc R U . . .
C38 C 0.3325(2) 0.07608(16) 0.71233(13) 0.0407(5) Uani 1 1 d . . . . .
H38 H 0.308435 -0.000366 0.702557 0.049 Uiso 1 1 calc R U . . .
C39 C 0.4070(2) 0.13755(17) 0.77597(13) 0.0396(5) Uani 1 1 d . . . . .
H39 H 0.432180 0.102547 0.809824 0.048 Uiso 1 1 calc R U . . .
C40 C 0.44648(18) 0.25082(16) 0.79194(11) 0.0314(4) Uani 1 1 d . . . . .
C41 C 0.28127(17) 0.28802(16) 0.62007(11) 0.0336(4) Uani 1 1 d . . . . .
H41 H 0.338557 0.366972 0.629137 0.040 Uiso 1 1 calc R U . . .
C42 C 0.2670(2) 0.2363(2) 0.54643(12) 0.0476(6) Uani 1 1 d . . . . .
H42A H 0.338724 0.232750 0.544566 0.071 Uiso 1 1 calc R U . . .
H42B H 0.250949 0.280692 0.514195 0.071 Uiso 1 1 calc R U . . .
H42C H 0.202242 0.162249 0.533342 0.071 Uiso 1 1 calc R U . . .
C43 C 0.1651(2) 0.2823(2) 0.62540(14) 0.0476(6) Uani 1 1 d . . . . .
H43A H 0.108509 0.205714 0.619592 0.071 Uiso 1 1 calc R U . . .
H43B H 0.135932 0.314560 0.589071 0.071 Uiso 1 1 calc R U . . .
H43C H 0.176660 0.322850 0.670939 0.071 Uiso 1 1 calc R U . . .
C44 C 0.52112(19) 0.31653(17) 0.86395(11) 0.0360(4) Uani 1 1 d . . . . .
H44 H 0.557834 0.395454 0.861025 0.043 Uiso 1 1 calc R U . . .
C45 C 0.6186(2) 0.2869(2) 0.89411(13) 0.0481(6) Uani 1 1 d . . . . .
H45A H 0.584798 0.210700 0.899584 0.072 Uiso 1 1 calc R U . . .
H45B H 0.666416 0.335004 0.939365 0.072 Uiso 1 1 calc R U . . .
H45C H 0.667076 0.295997 0.862688 0.072 Uiso 1 1 calc R U . . .
C46 C 0.4447(3) 0.3027(3) 0.91290(14) 0.0567(7) Uani 1 1 d . . . . .
H46A H 0.386384 0.327538 0.895250 0.085 Uiso 1 1 calc R U . . .
H46B H 0.493345 0.346244 0.959232 0.085 Uiso 1 1 calc R U . . .
H46C H 0.405467 0.225415 0.915448 0.085 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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
-1 0 1 0.0757
1 0 -1 0.0342
0 0 1 0.0181
0 0 -1 0.0342
0 -2 1 0.1133
0 2 -1 0.1184
-1 1 -2 0.1211
1 1 -2 0.0568
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
Cl1 C71 H71A 108.9 . . ?
Cl1 C71 H71B 108.9 . . ?
Cl2 C71 Cl1 113.53(18) . . ?
Cl2 C71 H71A 108.9 . . ?
Cl2 C71 H71B 108.9 . . ?
H71A C71 H71B 107.7 . . ?
C48 C47 C52 113.06(17) . . ?
C48 C47 B1 119.51(16) . . ?
C52 C47 B1 127.35(16) . . ?
F1 C48 C47 119.22(17) . . ?
F1 C48 C49 115.85(17) . . ?
C49 C48 C47 124.91(18) . . ?
F2 C49 C48 121.0(2) . . ?
F2 C49 C50 119.82(19) . . ?
C48 C49 C50 119.15(19) . . ?
F3 C50 C49 120.7(2) . . ?
F3 C50 C51 120.8(2) . . ?
C51 C50 C49 118.52(19) . . ?
F4 C51 C50 119.36(18) . . ?
F4 C51 C52 120.37(18) . . ?
C50 C51 C52 120.27(18) . . ?
F5 C52 C47 121.59(16) . . ?
F5 C52 C51 114.46(16) . . ?
C51 C52 C47 123.95(17) . . ?
C54 C53 C58 112.92(17) . . ?
C54 C53 B1 127.84(16) . . ?
C58 C53 B1 119.02(15) . . ?
F6 C54 C53 121.13(16) . . ?
F6 C54 C55 114.93(16) . . ?
C55 C54 C53 123.94(17) . . ?
F7 C55 C54 120.01(18) . . ?
F7 C55 C56 119.96(18) . . ?
C56 C55 C54 120.02(17) . . ?
F8 C56 C55 120.77(18) . . ?
F8 C56 C57 120.49(18) . . ?
C55 C56 C57 118.72(17) . . ?
F9 C57 C56 119.88(17) . . ?
F9 C57 C58 120.87(17) . . ?
C58 C57 C56 119.23(17) . . ?
F10 C58 C53 118.77(16) . . ?
F10 C58 C57 116.12(16) . . ?
C57 C58 C53 125.10(17) . . ?
C60 C59 B1 117.91(16) . . ?
C64 C59 C60 113.67(15) . . ?
C64 C59 B1 128.00(16) . . ?
F11 C60 C59 119.37(15) . . ?
F11 C60 C61 116.36(16) . . ?
C61 C60 C59 124.26(17) . . ?
F12 C61 C60 120.23(17) . . ?
F12 C61 C62 120.29(16) . . ?
C62 C61 C60 119.48(18) . . ?
F13 C62 C61 120.51(18) . . ?
F13 C62 C63 120.41(18) . . ?
C61 C62 C63 119.07(16) . . ?
F14 C63 C62 119.47(16) . . ?
F14 C63 C64 120.71(17) . . ?
C62 C63 C64 119.80(17) . . ?
F15 C64 C59 121.31(15) . . ?
F15 C64 C63 115.02(16) . . ?
C59 C64 C63 123.67(17) . . ?
C66 C65 C70 113.50(18) . . ?
C66 C65 B1 127.18(17) . . ?
C70 C65 B1 118.38(17) . . ?
F16 C66 C65 121.48(17) . . ?
F16 C66 C67 114.82(19) . . ?
C65 C66 C67 123.7(2) . . ?
F17 C67 C66 120.1(2) . . ?
F17 C67 C68 120.32(19) . . ?
C68 C67 C66 119.6(2) . . ?
F18 C68 C67 120.5(2) . . ?
F18 C68 C69 120.0(2) . . ?
C67 C68 C69 119.49(19) . . ?
F19 C69 C68 120.15(19) . . ?
F19 C69 C70 120.9(2) . . ?
C68 C69 C70 119.0(2) . . ?
F20 C70 C65 119.42(17) . . ?
F20 C70 C69 115.74(18) . . ?
C69 C70 C65 124.8(2) . . ?
C53 B1 C47 103.34(14) . . ?
C53 B1 C59 113.40(15) . . ?
C53 B1 C65 113.76(14) . . ?
C59 B1 C47 112.95(14) . . ?
C65 B1 C47 113.97(15) . . ?
C65 B1 C59 99.90(13) . . ?
C1 N1 C2 109.88(14) . . ?
C1 N1 C23 126.66(14) . . ?
C2 N1 C23 123.46(14) . . ?
C1 N2 C3 109.45(14) . . ?
C1 N2 C35 126.78(15) . . ?
C3 N2 C35 123.46(15) . . ?
N1 C1 C4 123.37(15) . . ?
N2 C1 N1 106.72(15) . . ?
N2 C1 C4 129.88(15) . . ?
N1 C2 H2 126.6 . . ?
C3 C2 N1 106.89(15) . . ?
C3 C2 H2 126.6 . . ?
N2 C3 H3 126.5 . . ?
C2 C3 N2 107.06(16) . . ?
C2 C3 H3 126.5 . . ?
C1 C4 H4 106.0 . . ?
C5 C4 C1 112.14(15) . . ?
C5 C4 H4 106.0 . . ?
C5 C4 C9 112.13(14) . . ?
C9 C4 C1 113.73(15) . . ?
C9 C4 H4 106.0 . . ?
C4 C5 H5 118.5 . . ?
C6 C5 C4 123.05(16) . . ?
C6 C5 H5 118.5 . . ?
C5 C6 H6 118.3 . . ?
C5 C6 C7 123.36(17) . . ?
C7 C6 H6 118.3 . . ?
C8 C7 C6 114.86(15) . . ?
C10 C7 C6 122.42(17) . . ?
C10 C7 C8 122.72(17) . . ?
C7 C8 H8 118.4 . . ?
C9 C8 C7 123.18(17) . . ?
C9 C8 H8 118.4 . . ?
C4 C9 H9 118.4 . . ?
C8 C9 C4 123.15(17) . . ?
C8 C9 H9 118.4 . . ?
C7 C10 C11 122.47(17) . . ?
C7 C10 C17 123.36(17) . . ?
C11 C10 C17 114.17(15) . . ?
C12 C11 C10 120.42(18) . . ?
C16 C11 C10 121.11(17) . . ?
C16 C11 C12 118.45(18) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.74(19) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.0(2) . . ?
C16 C15 H15 120.0 . . ?
C11 C16 H16 119.5 . . ?
C15 C16 C11 120.91(19) . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C10 119.3(2) . . ?
C22 C17 C10 122.5(2) . . ?
C22 C17 C18 118.1(2) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.6 . . ?
C20 C19 C18 120.7(3) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 120.3 . . ?
C19 C20 C21 119.3(2) . . ?
C21 C20 H20 120.3 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.2(3) . . ?
C22 C21 H21 119.9 . . ?
C17 C22 C21 120.7(3) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 N1 118.17(16) . . ?
C24 C23 C28 124.43(17) . . ?
C28 C23 N1 117.37(16) . . ?
C23 C24 C25 116.36(18) . . ?
C23 C24 C29 121.97(17) . . ?
C25 C24 C29 121.66(18) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.0(2) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 119.5 . . ?
C27 C26 C25 120.92(19) . . ?
C27 C26 H26 119.5 . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 120.99(19) . . ?
C28 C27 H27 119.5 . . ?
C23 C28 C32 122.13(16) . . ?
C27 C28 C23 116.22(18) . . ?
C27 C28 C32 121.64(17) . . ?
C24 C29 H29 107.5 . . ?
C30 C29 C24 112.6(2) . . ?
C30 C29 H29 107.5 . . ?
C30 C29 C31 111.3(2) . . ?
C31 C29 C24 110.28(18) . . ?
C31 C29 H29 107.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32 107.8 . . ?
C28 C32 C33 111.54(18) . . ?
C28 C32 C34 111.24(15) . . ?
C33 C32 H32 107.8 . . ?
C33 C32 C34 110.61(16) . . ?
C34 C32 H32 107.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N2 116.82(17) . . ?
C36 C35 C40 124.86(17) . . ?
C40 C35 N2 118.23(17) . . ?
C35 C36 C37 116.35(19) . . ?
C35 C36 C41 123.08(16) . . ?
C37 C36 C41 120.55(19) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 C36 120.7(2) . . ?
C38 C37 H37 119.6 . . ?
C37 C38 H38 119.5 . . ?
C39 C38 C37 120.99(19) . . ?
C39 C38 H38 119.5 . . ?
C38 C39 H39 119.4 . . ?
C38 C39 C40 121.3(2) . . ?
C40 C39 H39 119.4 . . ?
C35 C40 C39 115.7(2) . . ?
C35 C40 C44 123.29(17) . . ?
C39 C40 C44 120.9(2) . . ?
C36 C41 H41 107.7 . . ?
C36 C41 C42 112.50(17) . . ?
C36 C41 C43 111.21(19) . . ?
C42 C41 H41 107.7 . . ?
C42 C41 C43 109.77(19) . . ?
C43 C41 H41 107.7 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C44 H44 107.8 . . ?
C40 C44 C45 113.40(18) . . ?
C40 C44 C46 109.91(19) . . ?
C45 C44 H44 107.8 . . ?
C45 C44 C46 109.9(2) . . ?
C46 C44 H44 107.8 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
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
Cl1 C71 1.753(3) . ?
Cl2 C71 1.744(3) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
F1 C48 1.355(2) . ?
F2 C49 1.343(2) . ?
F3 C50 1.340(2) . ?
F4 C51 1.353(2) . ?
F5 C52 1.353(2) . ?
F6 C54 1.355(2) . ?
F7 C55 1.350(2) . ?
F8 C56 1.337(2) . ?
F9 C57 1.344(2) . ?
F10 C58 1.357(2) . ?
F11 C60 1.347(2) . ?
F12 C61 1.350(2) . ?
F13 C62 1.344(2) . ?
F14 C63 1.341(2) . ?
F15 C64 1.348(2) . ?
F16 C66 1.347(2) . ?
F17 C67 1.344(3) . ?
F18 C68 1.342(2) . ?
F19 C69 1.341(3) . ?
F20 C70 1.347(2) . ?
C47 C48 1.390(3) . ?
C47 C52 1.393(3) . ?
C47 B1 1.658(3) . ?
C48 C49 1.379(3) . ?
C49 C50 1.384(3) . ?
C50 C51 1.373(3) . ?
C51 C52 1.379(3) . ?
C53 C54 1.388(2) . ?
C53 C58 1.392(3) . ?
C53 B1 1.646(3) . ?
C54 C55 1.386(3) . ?
C55 C56 1.370(3) . ?
C56 C57 1.379(3) . ?
C57 C58 1.372(3) . ?
C59 C60 1.398(3) . ?
C59 C64 1.383(3) . ?
C59 B1 1.657(2) . ?
C60 C61 1.379(3) . ?
C61 C62 1.371(3) . ?
C62 C63 1.376(3) . ?
C63 C64 1.390(3) . ?
C65 C66 1.389(3) . ?
C65 C70 1.391(3) . ?
C65 B1 1.657(3) . ?
C66 C67 1.395(3) . ?
C67 C68 1.373(4) . ?
C68 C69 1.375(4) . ?
C69 C70 1.382(3) . ?
N1 C1 1.343(2) . ?
N1 C2 1.378(2) . ?
N1 C23 1.448(2) . ?
N2 C1 1.340(2) . ?
N2 C3 1.386(2) . ?
N2 C35 1.457(2) . ?
C1 C4 1.512(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.346(3) . ?
C3 H3 0.9500 . ?
C4 H4 1.0000 . ?
C4 C5 1.501(3) . ?
C4 C9 1.505(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.335(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.464(2) . ?
C7 C8 1.457(3) . ?
C7 C10 1.360(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.337(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.487(3) . ?
C10 C17 1.491(3) . ?
C11 C12 1.398(3) . ?
C11 C16 1.388(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.379(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(3) . ?
C17 C22 1.384(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.379(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.381(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.394(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.393(3) . ?
C23 C28 1.402(3) . ?
C24 C25 1.397(3) . ?
C24 C29 1.519(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.380(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.378(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.398(3) . ?
C28 C32 1.512(3) . ?
C29 H29 1.0000 . ?
C29 C30 1.507(3) . ?
C29 C31 1.518(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 1.0000 . ?
C32 C33 1.526(3) . ?
C32 C34 1.534(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.394(3) . ?
C35 C40 1.398(3) . ?
C36 C37 1.395(3) . ?
C36 C41 1.517(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.386(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.373(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.401(3) . ?
C40 C44 1.514(3) . ?
C41 H41 1.0000 . ?
C41 C42 1.530(3) . ?
C41 C43 1.536(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44 1.0000 . ?
C44 C45 1.530(3) . ?
C44 C46 1.537(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
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
F1 C48 C49 F2 0.8(3) . . . . ?
F1 C48 C49 C50 179.7(2) . . . . ?
F2 C49 C50 F3 0.7(4) . . . . ?
F2 C49 C50 C51 -179.4(2) . . . . ?
F3 C50 C51 F4 -0.8(3) . . . . ?
F3 C50 C51 C52 178.31(19) . . . . ?
F4 C51 C52 F5 -1.9(3) . . . . ?
F4 C51 C52 C47 177.72(17) . . . . ?
F6 C54 C55 F7 -0.6(3) . . . . ?
F6 C54 C55 C56 179.01(17) . . . . ?
F7 C55 C56 F8 -2.8(3) . . . . ?
F7 C55 C56 C57 178.89(17) . . . . ?
F8 C56 C57 F9 2.0(3) . . . . ?
F8 C56 C57 C58 -176.80(16) . . . . ?
F9 C57 C58 F10 -0.2(2) . . . . ?
F9 C57 C58 C53 -179.08(16) . . . . ?
F11 C60 C61 F12 -0.9(3) . . . . ?
F11 C60 C61 C62 179.61(17) . . . . ?
F12 C61 C62 F13 -1.7(3) . . . . ?
F12 C61 C62 C63 179.27(17) . . . . ?
F13 C62 C63 F14 0.5(3) . . . . ?
F13 C62 C63 C64 -177.84(17) . . . . ?
F14 C63 C64 F15 1.7(2) . . . . ?
F14 C63 C64 C59 -177.76(16) . . . . ?
F16 C66 C67 F17 1.1(3) . . . . ?
F16 C66 C67 C68 -177.35(16) . . . . ?
F17 C67 C68 F18 0.9(3) . . . . ?
F17 C67 C68 C69 -178.75(17) . . . . ?
F18 C68 C69 F19 1.0(3) . . . . ?
F18 C68 C69 C70 -179.76(17) . . . . ?
F19 C69 C70 F20 -1.6(3) . . . . ?
F19 C69 C70 C65 179.58(17) . . . . ?
C47 C48 C49 F2 -177.7(2) . . . . ?
C47 C48 C49 C50 1.2(3) . . . . ?
C48 C47 C52 F5 -176.52(17) . . . . ?
C48 C47 C52 C51 3.9(3) . . . . ?
C48 C47 B1 C53 68.1(2) . . . . ?
C48 C47 B1 C59 -168.96(17) . . . . ?
C48 C47 B1 C65 -55.8(2) . . . . ?
C48 C49 C50 F3 -178.2(2) . . . . ?
C48 C49 C50 C51 1.6(3) . . . . ?
C49 C50 C51 F4 179.31(19) . . . . ?
C49 C50 C51 C52 -1.6(3) . . . . ?
C50 C51 C52 F5 179.00(18) . . . . ?
C50 C51 C52 C47 -1.4(3) . . . . ?
C52 C47 C48 F1 177.78(17) . . . . ?
C52 C47 C48 C49 -3.8(3) . . . . ?
C52 C47 B1 C53 -108.4(2) . . . . ?
C52 C47 B1 C59 14.6(3) . . . . ?
C52 C47 B1 C65 127.69(19) . . . . ?
C53 C54 C55 F7 178.90(17) . . . . ?
C53 C54 C55 C56 -1.5(3) . . . . ?
C54 C53 C58 F10 179.38(15) . . . . ?
C54 C53 C58 C57 -1.7(3) . . . . ?
C54 C53 B1 C47 -108.3(2) . . . . ?
C54 C53 B1 C59 129.09(18) . . . . ?
C54 C53 B1 C65 15.8(3) . . . . ?
C54 C55 C56 F8 177.62(17) . . . . ?
C54 C55 C56 C57 -0.7(3) . . . . ?
C55 C56 C57 F9 -179.63(17) . . . . ?
C55 C56 C57 C58 1.5(3) . . . . ?
C56 C57 C58 F10 178.66(16) . . . . ?
C56 C57 C58 C53 -0.3(3) . . . . ?
C58 C53 C54 F6 -177.95(15) . . . . ?
C58 C53 C54 C55 2.6(3) . . . . ?
C58 C53 B1 C47 65.86(19) . . . . ?
C58 C53 B1 C59 -56.8(2) . . . . ?
C58 C53 B1 C65 -170.04(15) . . . . ?
C59 C60 C61 F12 178.95(17) . . . . ?
C59 C60 C61 C62 -0.6(3) . . . . ?
C60 C59 C64 F15 178.49(15) . . . . ?
C60 C59 C64 C63 -2.1(3) . . . . ?
C60 C59 B1 C47 53.9(2) . . . . ?
C60 C59 B1 C53 171.01(15) . . . . ?
C60 C59 B1 C65 -67.58(19) . . . . ?
C60 C61 C62 F13 177.85(17) . . . . ?
C60 C61 C62 C63 -1.2(3) . . . . ?
C61 C62 C63 F14 179.56(17) . . . . ?
C61 C62 C63 C64 1.2(3) . . . . ?
C62 C63 C64 F15 179.95(16) . . . . ?
C62 C63 C64 C59 0.5(3) . . . . ?
C64 C59 C60 F11 -178.01(15) . . . . ?
C64 C59 C60 C61 2.2(3) . . . . ?
C64 C59 B1 C47 -134.08(18) . . . . ?
C64 C59 B1 C53 -16.9(2) . . . . ?
C64 C59 B1 C65 104.5(2) . . . . ?
C65 C66 C67 F17 178.94(17) . . . . ?
C65 C66 C67 C68 0.5(3) . . . . ?
C66 C65 C70 F20 -179.00(15) . . . . ?
C66 C65 C70 C69 -0.2(3) . . . . ?
C66 C65 B1 C47 -16.9(2) . . . . ?
C66 C65 B1 C53 -135.06(18) . . . . ?
C66 C65 B1 C59 103.80(19) . . . . ?
C66 C67 C68 F18 179.34(17) . . . . ?
C66 C67 C68 C69 -0.4(3) . . . . ?
C67 C68 C69 F19 -179.30(17) . . . . ?
C67 C68 C69 C70 -0.1(3) . . . . ?
C68 C69 C70 F20 179.21(16) . . . . ?
C68 C69 C70 C65 0.3(3) . . . . ?
C70 C65 C66 F16 177.48(15) . . . . ?
C70 C65 C66 C67 -0.3(3) . . . . ?
C70 C65 B1 C47 174.98(15) . . . . ?
C70 C65 B1 C53 56.8(2) . . . . ?
C70 C65 B1 C59 -64.31(19) . . . . ?
B1 C47 C48 F1 0.8(3) . . . . ?
B1 C47 C48 C49 179.2(2) . . . . ?
B1 C47 C52 F5 0.1(3) . . . . ?
B1 C47 C52 C51 -179.43(18) . . . . ?
B1 C53 C54 F6 -3.5(3) . . . . ?
B1 C53 C54 C55 177.03(17) . . . . ?
B1 C53 C58 F10 4.4(2) . . . . ?
B1 C53 C58 C57 -176.70(16) . . . . ?
B1 C59 C60 F11 -4.9(2) . . . . ?
B1 C59 C60 C61 175.32(17) . . . . ?
B1 C59 C64 F15 6.2(3) . . . . ?
B1 C59 C64 C63 -174.46(17) . . . . ?
B1 C65 C66 F16 8.9(3) . . . . ?
B1 C65 C66 C67 -168.87(17) . . . . ?
B1 C65 C70 F20 -9.3(2) . . . . ?
B1 C65 C70 C69 169.52(17) . . . . ?
N1 C1 C4 C5 105.04(19) . . . . ?
N1 C1 C4 C9 -126.43(18) . . . . ?
N1 C2 C3 N2 -0.2(2) . . . . ?
N1 C23 C24 C25 177.70(16) . . . . ?
N1 C23 C24 C29 -0.9(3) . . . . ?
N1 C23 C28 C27 -176.01(15) . . . . ?
N1 C23 C28 C32 4.1(2) . . . . ?
N2 C1 C4 C5 -72.9(2) . . . . ?
N2 C1 C4 C9 55.6(3) . . . . ?
N2 C35 C36 C37 -178.96(17) . . . . ?
N2 C35 C36 C41 -0.3(3) . . . . ?
N2 C35 C40 C39 179.15(17) . . . . ?
N2 C35 C40 C44 3.2(3) . . . . ?
C1 N1 C2 C3 0.4(2) . . . . ?
C1 N1 C23 C24 83.4(2) . . . . ?
C1 N1 C23 C28 -98.7(2) . . . . ?
C1 N2 C3 C2 -0.1(2) . . . . ?
C1 N2 C35 C36 -86.6(2) . . . . ?
C1 N2 C35 C40 96.7(2) . . . . ?
C1 C4 C5 C6 134.66(19) . . . . ?
C1 C4 C9 C8 -134.41(19) . . . . ?
C2 N1 C1 N2 -0.5(2) . . . . ?
C2 N1 C1 C4 -178.88(16) . . . . ?
C2 N1 C23 C24 -96.1(2) . . . . ?
C2 N1 C23 C28 81.8(2) . . . . ?
C3 N2 C1 N1 0.4(2) . . . . ?
C3 N2 C1 C4 178.61(18) . . . . ?
C3 N2 C35 C36 86.3(2) . . . . ?
C3 N2 C35 C40 -90.4(2) . . . . ?
C4 C5 C6 C7 -2.4(3) . . . . ?
C5 C4 C9 C8 -5.9(3) . . . . ?
C5 C6 C7 C8 -0.6(3) . . . . ?
C5 C6 C7 C10 179.14(19) . . . . ?
C6 C7 C8 C9 0.0(3) . . . . ?
C6 C7 C10 C11 6.6(3) . . . . ?
C6 C7 C10 C17 -173.59(19) . . . . ?
C7 C8 C9 C4 3.5(3) . . . . ?
C7 C10 C11 C12 -127.0(2) . . . . ?
C7 C10 C11 C16 54.4(3) . . . . ?
C7 C10 C17 C18 -119.5(2) . . . . ?
C7 C10 C17 C22 64.2(3) . . . . ?
C8 C7 C10 C11 -173.68(18) . . . . ?
C8 C7 C10 C17 6.1(3) . . . . ?
C9 C4 C5 C6 5.3(3) . . . . ?
C10 C7 C8 C9 -179.7(2) . . . . ?
C10 C11 C12 C13 179.70(19) . . . . ?
C10 C11 C16 C15 -179.53(17) . . . . ?
C10 C17 C18 C19 -177.8(3) . . . . ?
C10 C17 C22 C21 176.3(2) . . . . ?
C11 C10 C17 C18 60.3(3) . . . . ?
C11 C10 C17 C22 -115.9(2) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
C12 C11 C16 C15 1.8(3) . . . . ?
C12 C13 C14 C15 1.3(3) . . . . ?
C13 C14 C15 C16 -1.2(3) . . . . ?
C14 C15 C16 C11 -0.4(3) . . . . ?
C16 C11 C12 C13 -1.7(3) . . . . ?
C17 C10 C11 C12 53.1(3) . . . . ?
C17 C10 C11 C16 -125.5(2) . . . . ?
C17 C18 C19 C20 1.3(5) . . . . ?
C18 C17 C22 C21 0.0(4) . . . . ?
C18 C19 C20 C21 0.2(5) . . . . ?
C19 C20 C21 C22 -1.5(5) . . . . ?
C20 C21 C22 C17 1.4(4) . . . . ?
C22 C17 C18 C19 -1.4(4) . . . . ?
C23 N1 C1 N2 179.94(16) . . . . ?
C23 N1 C1 C4 1.6(3) . . . . ?
C23 N1 C2 C3 -179.98(17) . . . . ?
C23 C24 C25 C26 -2.0(3) . . . . ?
C23 C24 C29 C30 -136.6(2) . . . . ?
C23 C24 C29 C31 98.4(3) . . . . ?
C23 C28 C32 C33 138.55(17) . . . . ?
C23 C28 C32 C34 -97.4(2) . . . . ?
C24 C23 C28 C27 1.8(3) . . . . ?
C24 C23 C28 C32 -178.14(17) . . . . ?
C24 C25 C26 C27 2.3(3) . . . . ?
C25 C24 C29 C30 44.8(3) . . . . ?
C25 C24 C29 C31 -80.2(3) . . . . ?
C25 C26 C27 C28 -0.4(3) . . . . ?
C26 C27 C28 C23 -1.5(3) . . . . ?
C26 C27 C28 C32 178.39(19) . . . . ?
C27 C28 C32 C33 -41.3(2) . . . . ?
C27 C28 C32 C34 82.7(2) . . . . ?
C28 C23 C24 C25 0.0(3) . . . . ?
C28 C23 C24 C29 -178.70(17) . . . . ?
C29 C24 C25 C26 176.7(2) . . . . ?
C35 N2 C1 N1 174.11(17) . . . . ?
C35 N2 C1 C4 -7.6(3) . . . . ?
C35 N2 C3 C2 -174.10(18) . . . . ?
C35 C36 C37 C38 0.2(3) . . . . ?
C35 C36 C41 C42 142.9(2) . . . . ?
C35 C36 C41 C43 -93.4(2) . . . . ?
C35 C40 C44 C45 -139.4(2) . . . . ?
C35 C40 C44 C46 97.2(2) . . . . ?
C36 C35 C40 C39 2.7(3) . . . . ?
C36 C35 C40 C44 -173.21(18) . . . . ?
C36 C37 C38 C39 1.6(3) . . . . ?
C37 C36 C41 C42 -38.5(3) . . . . ?
C37 C36 C41 C43 85.1(2) . . . . ?
C37 C38 C39 C40 -1.3(4) . . . . ?
C38 C39 C40 C35 -0.7(3) . . . . ?
C38 C39 C40 C44 175.3(2) . . . . ?
C39 C40 C44 C45 44.9(3) . . . . ?
C39 C40 C44 C46 -78.5(3) . . . . ?
C40 C35 C36 C37 -2.5(3) . . . . ?
C40 C35 C36 C41 176.16(18) . . . . ?
C41 C36 C37 C38 -178.4(2) . . . . ?
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
-1.0002 0.0006 1.0001 -0.1198 0.0460 -0.0410
1.0002 -0.0006 -1.0001 0.1198 -0.0460 0.0410
0.0005 -0.0004 1.0000 0.0047 0.0796 -0.0047
-0.0005 0.0004 -1.0000 -0.0047 -0.0796 0.0047
-0.0012 -1.9989 0.9997 -0.1638 0.0489 0.1799
0.0012 1.9989 -0.9997 0.1638 -0.0489 -0.1799
-1.0010 1.0010 -1.9997 -0.0497 -0.1773 -0.1193
1.0006 0.9990 -1.9999 0.1993 -0.1103 -0.0466
