#------------------------------------------------------------------------------
#$Date: 2019-11-17 15:18:17 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230810 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/63/7156331.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_7156331
loop_
_publ_author_name
'Wang, Denan'
'Ivanov, Maxim V.'
'Mirzaei, Saber'
'Lindeman, Sergey V.'
'Rathore, Rajendra'
_publ_section_title
;
 An electron-transfer induced conformational transformation: from
 non-cofacial "sofa" to cofacial "boat" in
 cyclotetraveratrylene (CTTV) and formation of charge transfer complexes.
;
_journal_issue                   31
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              5712
_journal_page_last               5717
_journal_paper_doi               10.1039/c8ob01118d
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety
'C8 Cl2 N2 O2, 2(C18 H20 O4), 3.23(C H Cl3), 0.77(C3 H7)'
_chemical_formula_sum            'C49.55 H48.64 Cl11.68 N2 O10'
_chemical_formula_weight         1246.20
_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     direct
_audit_creation_date             2018-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-17 deposited with the CCDC.
2018-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                111.109(4)
_cell_angle_beta                 94.141(4)
_cell_angle_gamma                100.255(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0667(4)
_cell_length_b                   16.1954(7)
_cell_length_c                   19.0021(8)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.4760
_cell_measurement_theta_min      4.4920
_cell_volume                     2812.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  31.00   1.00   10.00    --  -41.96  57.00 -90.00  101
  2  ω   -114.00 -14.00   1.00   10.00    --  -41.96 -57.00 120.00  100
  3  ω    -66.00  33.00   1.00   10.00    --  -41.96  37.00  60.00   99
  4  ω      1.00  83.00   1.00   10.00    --   41.96 -99.00   0.00   82
  5  ω     94.00 173.00   1.00   40.00    --  100.00 125.00 120.00   79
  6  ω     94.00 173.00   1.00   40.00    --  100.00 125.00   0.00   79
  7  ω     71.00 172.00   1.00   40.00    --  100.00  61.00  90.00  101
  8  ω     74.00 173.00   1.00   40.00    --  100.00  45.00  60.00   99
  9  ω     94.00 173.00   1.00   40.00    --  100.00 125.00 -30.00   79
 10  ω     27.00 121.00   1.00   40.00    --  100.00-125.00   0.00   94
 11  ω     71.00 172.00   1.00   40.00    --  100.00  61.00 -60.00  101
 12  ω     24.00 133.00   1.00   40.00    --  100.00 -77.00  30.00  109
 13  ω     27.00 121.00   1.00   40.00    --  100.00-125.00 -60.00   94
 14  ω     27.00 121.00   1.00   40.00    --  100.00-125.00  90.00   94
 15  ω     67.00 176.00   1.00   40.00    --  100.00  77.00 120.00  109
 16  ω     27.00 121.00   1.00   40.00    --  100.00-125.00-150.00   94
 17  ω     74.00 173.00   1.00   40.00    --  100.00  45.00-180.00   99
 18  ω   -114.00 -14.00   1.00   10.00    --  -41.96 -57.00-150.00  100
 19  ω   -118.00  -9.00   1.00   10.00    --  -41.96 -77.00  30.00  109
 20  ω   -118.00  -9.00   1.00   10.00    --  -41.96 -77.00 -60.00  109
 21  ω     71.00 172.00   1.00   40.00    --  100.00  61.00-150.00  101
 22  ω     71.00 172.00   1.00   40.00    --  100.00  61.00   0.00  101
 23  ω     71.00 172.00   1.00   40.00    --  100.00  61.00 -90.00  101
 24  ω     71.00 172.00   1.00   40.00    --  100.00  61.00  60.00  101
 25  ω     71.00 172.00   1.00   40.00    --  100.00  61.00 -30.00  101
 26  ω     71.00 172.00   1.00   40.00    --  100.00  61.00-180.00  101
 27  ω     67.00 176.00   1.00   40.00    --  100.00  77.00   0.00  109
 28  ω     71.00 172.00   1.00   40.00    --  100.00  61.00-120.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0499603000
_diffrn_orient_matrix_UB_12      -0.0324652000
_diffrn_orient_matrix_UB_13      -0.0781314000
_diffrn_orient_matrix_UB_21      0.0940453000
_diffrn_orient_matrix_UB_22      -0.0500304000
_diffrn_orient_matrix_UB_23      0.0289125000
_diffrn_orient_matrix_UB_31      -0.1157203000
_diffrn_orient_matrix_UB_32      -0.0858208000
_diffrn_orient_matrix_UB_33      -0.0279702000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52221
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        70.775
_diffrn_reflns_theta_max         70.775
_diffrn_reflns_theta_min         4.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.743
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             1277
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.017
_refine_diff_density_max         2.131
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         10686
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0664
_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)+(0.1359P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6636
_reflns_number_total             10686
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ob01118d3.cif
_cod_data_source_block           raj29d4
_cod_depositor_comments
'Adding full bibliography for 7156330--7156331.cif.'
_cod_database_code               7156331
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula
'(C7 H10 O2)4 C8 Cl2 O2 N2 (C H Cl3)3.5 (C6 H14)0.5'
_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.
;
_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. Rigid bond restraints
 Cl5Q, C2Q, Cl4Q, Cl6Q
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl4S, C2S, Cl5S, Cl6S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl7Q, C3Q, Cl8Q, Cl9Q
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl7S, C3S, Cl8S, Cl9S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1S, C1S, Cl2S, Cl3S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl12, C4S, Cl11, Cl13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11S, C12S, C13S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C2S) = Uanis(C2Q)
Uanis(Cl4S) = Uanis(Cl4Q)
Uanis(C3Q) = Uanis(C3S)
4. Same fragment restrains
{Cl1S, Cl2S, Cl3S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl4S, Cl5S, Cl6S, C2S}
{Cl1S, Cl2S, Cl3S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl4Q, Cl5Q, Cl6Q, C2Q}
{Cl1S, Cl2S, Cl3S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl7S, Cl8S, Cl9S, C3S}
{Cl1S, Cl2S, Cl3S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl7Q, Cl8Q, Cl9Q, C3Q}
{Cl1S, Cl2S, Cl3S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl11, Cl12, Cl13, C4S}
5. Others
 Sof(C11S)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12S)=Sof(H12A)=Sof(H12B)=
 Sof(C13S)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(Cl11)=Sof(Cl12)=Sof(Cl13)=Sof(C4S)=Sof(H4S)=FVAR(1)
 Sof(Cl4Q)=Sof(Cl5Q)=Sof(Cl6Q)=Sof(C2Q)=Sof(H2Q)=1-FVAR(2)
 Sof(Cl4S)=Sof(Cl5S)=Sof(Cl6S)=Sof(C2S)=Sof(H2S)=FVAR(2)
 Sof(Cl7Q)=Sof(Cl8Q)=Sof(Cl9Q)=Sof(C3Q)=Sof(H3Q)=1-FVAR(3)
 Sof(Cl7S)=Sof(Cl8S)=Sof(Cl9S)=Sof(C3S)=Sof(H3S)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C2Q(H2Q), C3S(H3S), C3Q(H3Q), C4S(H4S)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C12S(H12A,H12B),
 C13S(H13A,H13B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C22(H22), C25(H25), C32(H32), C35(H35), C42(H42), C45(H45)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C11S(H11A,H11B,H11C)
;
_olex2_date_sample_data_collection 2018-02-16
_olex2_date_sample_submission    2018-02-13
_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 2.023
_oxdiff_exptl_absorpt_empirical_full_min 0.714
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 17.5698° 
 around [-0.57 0.36 0.74] (reciprocal) or [-0.83 0.34 0.44] (direct)
;
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 0.14229(12) -0.00465(7) 0.30880(7) 0.0570(3) Uani 1 1 d . . . . .
Cl2 Cl 0.42704(13) 0.03694(8) 0.41439(6) 0.0587(3) Uani 1 1 d . . . . .
O1A O 0.6286(3) 0.1781(2) 0.39550(15) 0.0516(7) Uani 1 1 d . . . . .
O2A O 0.1572(3) 0.10131(19) 0.21267(15) 0.0509(7) Uani 1 1 d . . . . .
N1A N 0.7075(5) 0.3224(3) 0.2956(3) 0.0644(11) Uani 1 1 d . . . . .
N2A N 0.3523(5) 0.2627(3) 0.1580(2) 0.0639(10) Uani 1 1 d . . . . .
C1A C 0.5215(4) 0.1593(3) 0.3534(2) 0.0424(9) Uani 1 1 d . . . . .
C2A C 0.5031(4) 0.2047(2) 0.2991(2) 0.0414(8) Uani 1 1 d . . . . .
C3A C 0.3824(4) 0.1848(3) 0.2526(2) 0.0423(9) Uani 1 1 d . . . . .
C4A C 0.2627(4) 0.1177(3) 0.2541(2) 0.0444(9) Uani 1 1 d . . . . .
C5A C 0.2823(4) 0.0723(3) 0.3088(2) 0.0446(9) Uani 1 1 d . . . . .
C6A C 0.4022(5) 0.0901(3) 0.3532(2) 0.0465(9) Uani 1 1 d . . . . .
C7A C 0.6193(5) 0.2703(3) 0.2976(2) 0.0479(9) Uani 1 1 d . . . . .
C8A C 0.3653(5) 0.2284(3) 0.2000(2) 0.0485(10) Uani 1 1 d . . . . .
O1 O -0.0825(3) -0.2987(2) -0.06152(17) 0.0535(7) Uani 1 1 d . . . . .
O2 O -0.1244(3) -0.1485(2) 0.03648(16) 0.0514(7) Uani 1 1 d . . . . .
O3 O 0.5044(3) -0.07997(17) 0.23740(14) 0.0428(6) Uani 1 1 d . . . . .
O4 O 0.7336(3) 0.03666(17) 0.27213(14) 0.0419(6) Uani 1 1 d . . . . .
C1 C 0.3876(4) -0.1496(2) -0.0725(2) 0.0393(8) Uani 1 1 d . . . . .
H1A H 0.384562 -0.213035 -0.106183 0.047 Uiso 1 1 calc R . . . .
H1B H 0.459374 -0.132934 -0.028293 0.047 Uiso 1 1 calc R . . . .
C2 C 0.3330(4) 0.0233(2) 0.03900(19) 0.0376(8) Uani 1 1 d . . . . .
H2A H 0.286637 0.073977 0.060489 0.045 Uiso 1 1 calc R . . . .
H2B H 0.375544 0.031489 -0.004078 0.045 Uiso 1 1 calc R . . . .
C11 C 0.2517(4) -0.1453(2) -0.04367(18) 0.0380(8) Uani 1 1 d . . . . .
C12 C 0.1481(4) -0.2242(2) -0.0677(2) 0.0407(8) Uani 1 1 d . . . . .
H12 H 0.163506 -0.279121 -0.103146 0.049 Uiso 1 1 calc R . . . .
C13 C 0.0229(4) -0.2240(3) -0.0408(2) 0.0448(9) Uani 1 1 d . . . . .
C14 C -0.0002(4) -0.1438(3) 0.0108(2) 0.0429(9) Uani 1 1 d . . . . .
C15 C 0.1006(4) -0.0653(3) 0.0346(2) 0.0412(8) Uani 1 1 d . . . . .
H15 H 0.083679 -0.010599 0.069755 0.049 Uiso 1 1 calc R . . . .
C16 C 0.2267(4) -0.0644(2) 0.00838(18) 0.0375(8) Uani 1 1 d . . . . .
C17 C -0.0548(5) -0.3847(3) -0.1052(2) 0.0561(11) Uani 1 1 d . . . . .
H17A H -0.030997 -0.384751 -0.154332 0.084 Uiso 1 1 calc GR . . . .
H17B H -0.135957 -0.432650 -0.113948 0.084 Uiso 1 1 calc GR . . . .
H17C H 0.021567 -0.395546 -0.077256 0.084 Uiso 1 1 calc GR . . . .
C18 C -0.1364(5) -0.0722(3) 0.1016(3) 0.0554(11) Uani 1 1 d . . . . .
H18A H -0.126221 -0.018244 0.088648 0.083 Uiso 1 1 calc GR . . . .
H18B H -0.064935 -0.061733 0.143654 0.083 Uiso 1 1 calc GR . . . .
H18C H -0.226206 -0.084206 0.117171 0.083 Uiso 1 1 calc GR . . . .
C21 C 0.4452(4) 0.0298(2) 0.09990(18) 0.0364(8) Uani 1 1 d . . . . .
C22 C 0.4207(4) -0.0271(2) 0.14076(19) 0.0368(8) Uani 1 1 d . . . . .
H22 H 0.334823 -0.068262 0.129530 0.044 Uiso 1 1 calc R . . . .
C23 C 0.5189(4) -0.0248(2) 0.19719(19) 0.0375(8) Uani 1 1 d . . . . .
C24 C 0.6447(4) 0.0379(2) 0.21510(19) 0.0369(8) Uani 1 1 d . . . . .
C25 C 0.6701(4) 0.0919(2) 0.17388(19) 0.0371(8) Uani 1 1 d . . . . .
H25 H 0.756576 0.132325 0.184783 0.044 Uiso 1 1 calc R . . . .
C26 C 0.5716(4) 0.0890(2) 0.11576(18) 0.0363(8) Uani 1 1 d . . . . .
C27 C 0.3808(4) -0.1485(3) 0.2172(2) 0.0475(9) Uani 1 1 d . . . . .
H27A H 0.369642 -0.186628 0.162815 0.071 Uiso 1 1 calc GR . . . .
H27B H 0.302865 -0.119517 0.227495 0.071 Uiso 1 1 calc GR . . . .
H27C H 0.385403 -0.186031 0.247416 0.071 Uiso 1 1 calc GR . . . .
C28 C 0.8581(4) 0.1039(3) 0.2962(2) 0.0479(9) Uani 1 1 d . . . . .
H28A H 0.908108 0.097647 0.252818 0.072 Uiso 1 1 calc GR . . . .
H28B H 0.914032 0.095845 0.336628 0.072 Uiso 1 1 calc GR . . . .
H28C H 0.837683 0.164389 0.315621 0.072 Uiso 1 1 calc GR . . . .
O5 O 0.1313(3) 0.21159(18) 0.42205(15) 0.0445(6) Uani 1 1 d . . . . .
O6 O 0.0721(3) 0.27248(19) 0.31886(15) 0.0466(6) Uani 1 1 d . . . . .
O7 O 0.2455(3) 0.7409(2) 0.33212(16) 0.0513(7) Uani 1 1 d . . . . .
O8 O 0.3563(3) 0.6419(2) 0.22291(16) 0.0556(8) Uani 1 1 d . . . . .
C3 C 0.6037(4) 0.3995(2) 0.49256(18) 0.0368(8) Uani 1 1 d . . . . .
H3A H 0.663672 0.362694 0.462446 0.044 Uiso 1 1 calc R . . . .
H3B H 0.641338 0.463644 0.500860 0.044 Uiso 1 1 calc R . . . .
C4 C 0.5204(4) 0.4835(2) 0.3803(2) 0.0377(8) Uani 1 1 d . . . . .
H4A H 0.562238 0.457376 0.333963 0.045 Uiso 1 1 calc R . . . .
H4B H 0.594807 0.513140 0.424136 0.045 Uiso 1 1 calc R . . . .
C31 C 0.4619(4) 0.3701(2) 0.44595(18) 0.0350(7) Uani 1 1 d . . . . .
C32 C 0.3638(4) 0.3040(2) 0.45572(18) 0.0377(8) Uani 1 1 d . . . . .
H32 H 0.387015 0.278928 0.491859 0.045 Uiso 1 1 calc R . . . .
C33 C 0.2344(4) 0.2740(2) 0.4146(2) 0.0386(8) Uani 1 1 d . . . . .
C34 C 0.2004(4) 0.3077(2) 0.3586(2) 0.0406(8) Uani 1 1 d . . . . .
C35 C 0.2964(4) 0.3741(2) 0.34923(19) 0.0390(8) Uani 1 1 d . . . . .
H35 H 0.273113 0.397677 0.312039 0.047 Uiso 1 1 calc R . . . .
C36 C 0.4266(4) 0.4078(2) 0.39262(19) 0.0364(8) Uani 1 1 d . . . . .
C37 C 0.1530(5) 0.1847(3) 0.4851(2) 0.0490(10) Uani 1 1 d . . . . .
H37A H 0.226310 0.151208 0.478034 0.074 Uiso 1 1 calc GR . . . .
H37B H 0.068846 0.145703 0.487950 0.074 Uiso 1 1 calc GR . . . .
H37C H 0.178807 0.238657 0.532433 0.074 Uiso 1 1 calc GR . . . .
C38 C 0.0371(5) 0.3035(3) 0.2596(2) 0.0526(10) Uani 1 1 d . . . . .
H38A H 0.099899 0.289608 0.222049 0.079 Uiso 1 1 calc GR . . . .
H38B H 0.044079 0.369193 0.281762 0.079 Uiso 1 1 calc GR . . . .
H38C H -0.056597 0.272916 0.234608 0.079 Uiso 1 1 calc GR . . . .
C41 C 0.4479(4) 0.5547(2) 0.37137(19) 0.0364(8) Uani 1 1 d . . . . .
C42 C 0.4375(4) 0.5651(2) 0.3008(2) 0.0410(8) Uani 1 1 d . . . . .
H42 H 0.477103 0.528525 0.260319 0.049 Uiso 1 1 calc R . . . .
C43 C 0.3704(4) 0.6276(3) 0.2899(2) 0.0430(9) Uani 1 1 d . . . . .
C44 C 0.3118(4) 0.6815(2) 0.3486(2) 0.0414(8) Uani 1 1 d . . . . .
C45 C 0.3233(4) 0.6728(2) 0.4188(2) 0.0388(8) Uani 1 1 d . . . . .
H45 H 0.284626 0.710077 0.459351 0.047 Uiso 1 1 calc R . . . .
C46 C 0.3916(4) 0.6094(2) 0.43023(19) 0.0364(8) Uani 1 1 d . . . . .
C47 C 0.4364(7) 0.5992(4) 0.1665(3) 0.0757(16) Uani 1 1 d . . . . .
H47A H 0.423076 0.616831 0.122710 0.113 Uiso 1 1 calc GR . . . .
H47B H 0.407613 0.533122 0.149665 0.113 Uiso 1 1 calc GR . . . .
H47C H 0.533132 0.618470 0.188601 0.113 Uiso 1 1 calc GR . . . .
C48 C 0.1911(6) 0.8004(3) 0.3927(3) 0.0641(13) Uani 1 1 d . . . . .
H48A H 0.152149 0.842006 0.374949 0.096 Uiso 1 1 calc GR . . . .
H48B H 0.264144 0.835349 0.435718 0.096 Uiso 1 1 calc GR . . . .
H48C H 0.119742 0.764777 0.409082 0.096 Uiso 1 1 calc GR . . . .
Cl1S Cl 0.40243(12) 0.16992(8) 0.62441(6) 0.0623(3) Uani 1 1 d D U . . .
Cl2S Cl 0.17937(17) 0.01258(9) 0.55791(7) 0.0848(5) Uani 1 1 d D U . . .
Cl3S Cl 0.16951(19) 0.15483(12) 0.70049(12) 0.1000(5) Uani 1 1 d D U . . .
C1S C 0.2752(4) 0.0951(3) 0.6431(2) 0.0519(10) Uani 1 1 d D U . . .
H1S H 0.320159 0.063499 0.671320 0.062 Uiso 1 1 calc R . . . .
Cl4S Cl 0.015(2) 0.7605(8) 0.1527(15) 0.0824(15) Uani 0.68(2) 1 d D U P A 1
Cl5S Cl -0.0621(5) 0.6021(3) 0.1872(4) 0.1104(14) Uani 0.68(2) 1 d D U P A 1
Cl6S Cl 0.1085(10) 0.6009(3) 0.0721(2) 0.0945(17) Uani 0.68(2) 1 d D U P A 1
C2S C 0.0647(15) 0.6667(7) 0.1598(7) 0.0721(19) Uani 0.68(2) 1 d D U P A 1
H2S H 0.147465 0.688286 0.199485 0.087 Uiso 0.68(2) 1 calc R . P A 1
Cl4Q Cl 0.030(5) 0.7674(18) 0.152(3) 0.0824(15) Uani 0.32(2) 1 d D U P A 2
Cl5Q Cl -0.0489(13) 0.5844(9) 0.139(2) 0.160(10) Uani 0.32(2) 1 d D U P A 2
Cl6Q Cl 0.171(2) 0.636(2) 0.0634(6) 0.134(7) Uani 0.32(2) 1 d D U P A 2
C2Q C 0.088(3) 0.6700(14) 0.1441(16) 0.0721(19) Uani 0.32(2) 1 d D U P A 2
H2Q H 0.154321 0.683742 0.190636 0.087 Uiso 0.32(2) 1 calc R . P A 2
Cl7S Cl 0.3299(8) 0.3962(4) -0.0225(4) 0.0752(12) Uani 0.701(6) 1 d D U P B 1
Cl8S Cl 0.4469(3) 0.23781(14) -0.06030(14) 0.0749(7) Uani 0.701(6) 1 d D U P B
1
Cl9S Cl 0.5482(3) 0.38852(14) 0.0795(2) 0.0831(8) Uani 0.701(6) 1 d D U P B 1
C3S C 0.4020(8) 0.3254(5) 0.0139(4) 0.0601(16) Uani 0.701(6) 1 d D U P B 1
H3S H 0.334042 0.298418 0.039906 0.072 Uiso 0.701(6) 1 calc R . P B 1
Cl7Q Cl 0.3074(17) 0.4120(8) -0.0248(9) 0.082(3) Uani 0.299(6) 1 d D U P B 2
Cl8Q Cl 0.3599(11) 0.2445(4) -0.1144(6) 0.143(5) Uani 0.299(6) 1 d D U P B 2
Cl9Q Cl 0.5266(9) 0.3475(10) 0.0273(8) 0.155(5) Uani 0.299(6) 1 d D U P B 2
C3Q C 0.3626(16) 0.3180(10) -0.0203(8) 0.0601(16) Uani 0.299(6) 1 d D U P B 2
H3Q H 0.299364 0.287272 0.005487 0.072 Uiso 0.299(6) 1 calc R . P B 2
Cl11 Cl -0.2402(7) 0.4540(4) 0.2061(4) 0.084(2) Uani 0.226(3) 1 d D U P C 1
Cl12 Cl -0.2079(6) 0.6222(4) 0.3276(5) 0.091(3) Uani 0.226(3) 1 d D U P C 1
Cl13 Cl 0.0239(6) 0.5421(4) 0.3017(6) 0.103(3) Uani 0.226(3) 1 d D U P C 1
C4S C -0.1536(14) 0.5197(10) 0.2972(10) 0.073(6) Uani 0.226(3) 1 d D U P C 1
H4S H -0.179085 0.487582 0.332047 0.087 Uiso 0.226(3) 1 calc R . P C 1
C11S C -0.0718(9) 0.5580(6) 0.3669(5) 0.088(2) Uani 0.774(3) 1 d . U P C 2
H11A H -0.117064 0.603220 0.358641 0.132 Uiso 0.774(3) 1 calc GR . P C 2
H11B H -0.126350 0.497004 0.336557 0.132 Uiso 0.774(3) 1 calc GR . P C 2
H11C H 0.018980 0.564406 0.351454 0.132 Uiso 0.774(3) 1 calc GR . P C 2
C12S C -0.0582(9) 0.5723(6) 0.4502(6) 0.094(2) Uani 0.774(3) 1 d . U P C 2
H12A H 0.005267 0.630949 0.480814 0.113 Uiso 0.774(3) 1 calc R . P C 2
H12B H -0.148127 0.573596 0.467950 0.113 Uiso 0.774(3) 1 calc R . P C 2
C13S C -0.0041(9) 0.4956(8) 0.4599(5) 0.098(3) Uani 0.774(3) 1 d . U P C 2
H13A H -0.065120 0.436984 0.426871 0.117 Uiso 0.774(3) 1 calc R . P C 2
H13B H 0.087651 0.496387 0.444296 0.117 Uiso 0.774(3) 1 calc R . P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 8 -11 0.0160
1 -8 11 0.0010
5 -2 -7 0.0481
-5 2 7 0.0481
-6 -2 5 0.0470
6 2 -5 0.0470
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
O1A C1A C2A 121.4(4) . .
O1A C1A C6A 122.3(4) . .
C2A C1A C6A 116.3(3) . .
C3A C2A C1A 121.6(4) . .
C3A C2A C7A 121.7(4) . .
C7A C2A C1A 116.8(4) . .
C2A C3A C4A 121.9(3) . .
C2A C3A C8A 121.4(4) . .
C8A C3A C4A 116.7(4) . .
O2A C4A C3A 120.8(4) . .
O2A C4A C5A 123.1(4) . .
C3A C4A C5A 116.1(3) . .
C4A C5A Cl1 114.8(3) . .
C6A C5A Cl1 123.2(3) . .
C6A C5A C4A 122.0(4) . .
C1A C6A Cl2 115.5(3) . .
C5A C6A Cl2 122.5(3) . .
C5A C6A C1A 122.0(4) . .
N1A C7A C2A 178.2(5) . .
N2A C8A C3A 179.5(5) . .
C13 O1 C17 117.2(3) . .
C14 O2 C18 116.2(3) . .
C23 O3 C27 117.3(3) . .
C24 O4 C28 116.8(3) . .
C11 C1 C26 115.4(3) . 2_655
C16 C2 C21 115.2(3) . .
C12 C11 C1 119.7(3) . .
C12 C11 C16 118.4(4) . .
C16 C11 C1 121.8(3) . .
C13 C12 C11 121.6(3) . .
O1 C13 C12 124.6(4) . .
O1 C13 C14 116.0(4) . .
C14 C13 C12 119.3(4) . .
O2 C14 C13 116.5(4) . .
O2 C14 C15 123.7(3) . .
C15 C14 C13 119.8(4) . .
C14 C15 C16 121.6(3) . .
C11 C16 C2 122.3(3) . .
C15 C16 C2 118.4(3) . .
C15 C16 C11 119.2(3) . .
C22 C21 C2 118.7(3) . .
C26 C21 C2 122.3(3) . .
C26 C21 C22 119.0(3) . .
C23 C22 C21 121.7(3) . .
O3 C23 C22 125.1(3) . .
O3 C23 C24 115.9(3) . .
C22 C23 C24 118.9(3) . .
O4 C24 C23 114.9(3) . .
O4 C24 C25 125.7(3) . .
C25 C24 C23 119.4(3) . .
C24 C25 C26 121.9(3) . .
C21 C26 C1 123.7(3) . 2_655
C21 C26 C25 118.9(3) . .
C25 C26 C1 117.3(3) . 2_655
C33 O5 C37 117.0(3) . .
C34 O6 C38 116.9(3) . .
C44 O7 C48 117.2(3) . .
C43 O8 C47 116.3(3) . .
C46 C3 C31 114.8(3) 2_666 .
C36 C4 C41 113.2(3) . .
C32 C31 C3 119.4(3) . .
C32 C31 C36 118.8(3) . .
C36 C31 C3 121.7(3) . .
C33 C32 C31 122.1(3) . .
O5 C33 C32 125.9(3) . .
O5 C33 C34 114.6(3) . .
C32 C33 C34 119.6(4) . .
O6 C34 C33 116.0(3) . .
O6 C34 C35 125.3(3) . .
C35 C34 C33 118.7(3) . .
C34 C35 C36 122.3(3) . .
C31 C36 C4 123.9(3) . .
C35 C36 C4 117.7(3) . .
C35 C36 C31 118.4(3) . .
C42 C41 C4 118.9(3) . .
C46 C41 C4 122.1(3) . .
C46 C41 C42 119.0(3) . .
C43 C42 C41 120.8(4) . .
O8 C43 C42 124.2(4) . .
O8 C43 C44 115.5(3) . .
C42 C43 C44 120.3(3) . .
O7 C44 C43 116.2(3) . .
O7 C44 C45 124.4(4) . .
C43 C44 C45 119.4(3) . .
C44 C45 C46 120.5(4) . .
C41 C46 C3 121.8(3) . 2_666
C41 C46 C45 120.0(3) . .
C45 C46 C3 118.1(3) . 2_666
Cl1S C1S Cl2S 111.1(2) . .
Cl3S C1S Cl1S 110.1(2) . .
Cl3S C1S Cl2S 110.6(2) . .
Cl4S C2S Cl5S 111.5(8) . .
Cl4S C2S Cl6S 109.7(8) . .
Cl5S C2S Cl6S 110.6(5) . .
Cl4Q C2Q Cl5Q 109.8(16) . .
Cl4Q C2Q Cl6Q 109.6(16) . .
Cl5Q C2Q Cl6Q 110.9(12) . .
Cl8S C3S Cl7S 110.3(4) . .
Cl9S C3S Cl7S 109.9(4) . .
Cl9S C3S Cl8S 108.8(4) . .
Cl7Q C3Q Cl8Q 106.8(9) . .
Cl9Q C3Q Cl7Q 111.6(10) . .
Cl9Q C3Q Cl8Q 108.7(10) . .
Cl11 C4S Cl12 107.4(9) . .
Cl11 C4S Cl13 113.5(10) . .
Cl13 C4S Cl12 109.4(8) . .
C13S C12S C11S 108.4(7) . .
C13S C13S C12S 110.2(10) 2_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 C5A 1.707(4) .
Cl2 C6A 1.707(4) .
O1A C1A 1.216(5) .
O2A C4A 1.202(5) .
N1A C7A 1.123(6) .
N2A C8A 1.137(6) .
C1A C2A 1.486(5) .
C1A C6A 1.488(6) .
C2A C3A 1.364(6) .
C2A C7A 1.444(6) .
C3A C4A 1.481(6) .
C3A C8A 1.434(6) .
C4A C5A 1.494(6) .
C5A C6A 1.344(6) .
O1 C13 1.372(5) .
O1 C17 1.430(5) .
O2 C14 1.374(5) .
O2 C18 1.431(5) .
O3 C23 1.365(4) .
O3 C27 1.435(5) .
O4 C24 1.364(4) .
O4 C28 1.428(5) .
C1 C11 1.512(6) .
C1 C26 1.515(5) 2_655
C2 C16 1.507(5) .
C2 C21 1.520(5) .
C11 C12 1.402(5) .
C11 C16 1.407(5) .
C12 C13 1.393(6) .
C13 C14 1.387(6) .
C14 C15 1.382(6) .
C15 C16 1.397(6) .
C21 C22 1.406(5) .
C21 C26 1.390(6) .
C22 C23 1.390(5) .
C23 C24 1.408(5) .
C24 C25 1.373(5) .
C25 C26 1.412(5) .
O5 C33 1.367(5) .
O5 C37 1.430(5) .
O6 C34 1.361(5) .
O6 C38 1.434(5) .
O7 C44 1.372(5) .
O7 C48 1.426(6) .
O8 C43 1.375(4) .
O8 C47 1.438(6) .
C3 C31 1.523(5) .
C3 C46 1.523(5) 2_666
C4 C36 1.509(5) .
C4 C41 1.521(5) .
C31 C32 1.396(5) .
C31 C36 1.412(5) .
C32 C33 1.378(5) .
C33 C34 1.406(5) .
C34 C35 1.385(6) .
C35 C36 1.400(5) .
C41 C42 1.408(5) .
C41 C46 1.384(5) .
C42 C43 1.378(6) .
C43 C44 1.389(6) .
C44 C45 1.391(5) .
C45 C46 1.401(5) .
Cl1S C1S 1.749(4) .
Cl2S C1S 1.758(4) .
Cl3S C1S 1.741(5) .
Cl4S C2S 1.729(9) .
Cl5S C2S 1.735(9) .
Cl6S C2S 1.761(9) .
Cl4Q C2Q 1.737(14) .
Cl5Q C2Q 1.738(15) .
Cl6Q C2Q 1.759(14) .
Cl7S C3S 1.767(7) .
Cl8S C3S 1.756(7) .
Cl9S C3S 1.745(7) .
Cl7Q C3Q 1.738(13) .
Cl8Q C3Q 1.751(13) .
Cl9Q C3Q 1.721(13) .
Cl11 C4S 1.736(14) .
Cl12 C4S 1.752(13) .
Cl13 C4S 1.748(13) .
C11S C12S 1.506(13) .
C12S C13S 1.505(14) .
C13S C13S 1.472(17) 2_566
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
-1.1546 7.6222 -11.1874 0.5690 -0.8134 -0.2076
1.1546 -7.6222 11.1874 -0.5690 0.8134 0.2076
4.8799 -1.9976 -7.2948 0.8786 0.3480 -0.1892
-4.8799 1.9976 7.2948 -0.8786 -0.3480 0.1892
-5.5813 -2.4531 4.9949 -0.5895 -0.2577 0.7167
5.5813 2.4531 -4.9949 0.5895 0.2577 -0.7167
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6377 50635 1814 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3623 50416 1814 nmt 0.9563 -0.1087 0.0174 0.3360 1.0848 0.2148 -0.3516
-0.2771 0.8693
