#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:00:42 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295180 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/23/1572341.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_1572341
loop_
_publ_author_name
'Judge, Neil R.'
'Hevia, Eva'
_publ_section_title
;
 Combining two relatively weak bases (Zn(TMP)₂ and
 KOtBu) for the regioselective metalation of non-activated arenes
 and heteroarenes.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14757
_journal_page_last               14765
_journal_paper_doi               10.1039/d4sc03892d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C42 H92 K2 N6 O4 Zn2'
_chemical_formula_sum            'C42 H92 K2 N6 O4 Zn2'
_chemical_formula_weight         954.15
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-20T13:55:28-00:00
_audit_update_record
;
2024-05-26 deposited with the CCDC.	2024-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                112.4692(14)
_cell_angle_beta                 92.8879(12)
_cell_angle_gamma                107.7984(13)
_cell_formula_units_Z            1
_cell_length_a                   10.92429(16)
_cell_length_b                   11.04872(16)
_cell_length_c                   13.15156(19)
_cell_measurement_reflns_used    46157
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      79.676
_cell_measurement_theta_min      3.699
_cell_volume                     1371.22(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -95.00  -6.00   1.00    0.50    --  -23.00 -63.00 -29.00   89
  2  ω    -40.00  50.00   1.00    0.50    --  -23.00  63.00 107.00   90
  3  ω     31.00 120.00   1.00    0.50    --   47.95  63.00 107.00   89
  4  ω     96.00 177.00   1.00    4.00    --  113.25  63.00 107.00   81
  5  ω     42.00  71.00   1.00    4.00    --  113.25 -63.00 -29.00   29
  6  ω    -70.00 -12.00   1.00    0.50    --  -23.00 125.00  60.00   58
  7  ω    -95.00   0.00   1.00    0.50    --  -23.00 -77.00 150.00   95
  8  ω    -95.00 -10.00   1.00    0.50    --  -23.00 -45.00 150.00   85
  9  ω      9.00  42.00   1.00    0.50    --   38.00  91.00 116.34   33
 10  ω     15.00  43.00   1.00    0.50    --   42.00  87.00-179.86   28
 11  ω     17.00  43.00   1.00    0.50    --   46.00  90.00  59.44   26
 12  ω     17.00  43.00   1.00    0.50    --   46.00  90.00 -88.97   26
 13  ω     -1.00  81.00   1.00    0.50    --   47.95 -99.00 -60.00   82
 14  ω    -24.00  65.00   1.00    0.50    --   47.95 -63.00 -29.00   89
 15  ω     29.00 122.00   1.00    0.50    --   50.00  74.00  32.18   93
 16  ω     28.00 122.00   1.00    0.50    --   50.00  76.00  -1.45   94
 17  ω     35.00 131.00   1.00    0.50    --   58.00  77.00  60.28   96
 18  ω     35.00 131.00   1.00    0.50    --   58.00  77.00  84.38   96
 19  ω     39.00 135.00   1.00    0.50    --   62.00  77.00-170.00   96
 20  ω     41.00 135.00   1.00    0.50    --   62.00  73.00 -23.90   94
 21  ω     40.00 135.00   1.00    0.50    --   62.00  75.00 -85.32   95
 22  ω     39.00 135.00   1.00    0.50    --   62.00  77.00-142.50   96
 23  ω     40.00 135.00   1.00    0.50    --   62.00  76.00 120.28   95
 24  ω     44.00 139.00   1.00    0.50    --   66.00  76.00 145.95   95
 25  ω     44.00 139.00   1.00    0.50    --   66.00  75.00 -59.02   95
 26  ω     44.00 139.00   1.00    0.50    --   66.00  76.00-119.05   95
 27  ω     44.00 139.00   1.00    0.50    --   66.00  76.00  10.67   95
 28  ω     51.00 143.00   1.00    0.50    --   70.00  67.00 105.25   92
 29  ω     47.00 143.00   1.00    0.50    --   70.00  77.00  51.05   96
 30  ω     51.00 143.00   1.00    0.50    --   70.00  69.00 174.14   92
 31  ω     48.00 143.00   1.00    0.50    --   70.00  75.00 -19.04   95
 32  ω     57.00 146.00   1.00    0.50    --   74.00  64.00-110.73   89
 33  ω     55.00 146.00   1.00    0.50    --   74.00  69.00  63.40   91
 34  ω     55.00 146.00   1.00    0.50    --   74.00  69.00 121.36   91
 35  ω     59.00 151.00   1.00    0.50    --   78.00  67.00 -53.21   92
 36  ω     62.00 150.00   1.00    0.50    --   78.00  60.00 -58.94   88
 37  ω     55.00 151.00   1.00    0.50    --   78.00  77.00   3.36   96
 38  ω     62.00 154.00   1.00    4.00    --   82.00  71.00  23.37   92
 39  ω     64.00 159.00   1.00    4.00    --   86.00  76.00-177.58   95
 40  ω     70.00 162.00   1.00    4.00    --   90.00  71.00 -41.47   92
 41  ω     80.00 170.00   1.00    4.00    --   98.00  65.00  60.01   90
 42  ω     86.00 175.00   1.00    4.00    --  102.00  61.00  -1.43   89
 43  ω    136.00 173.00   1.00    4.00    --  113.25  77.00-120.00   37
 44  ω    142.00 171.00   1.00    4.00    --  113.25  61.00  90.00   29
 45  ω     53.00 103.00   1.00    4.00    --  113.25 -94.00 150.00   50
 46  ω     99.00 127.00   1.00    4.00    --  113.25  61.00  90.00   28
 47  ω     91.00 176.00   1.00    4.00    --  113.25  77.00   0.00   85
 48  ω     44.00 106.00   1.00    4.00    --  113.25 -94.00 -30.00   62
 49  ω     97.00 175.00   1.00    4.00    --  113.25  61.00 150.00   78
 50  ω    135.00 170.00   1.00    4.00    --  113.25  61.00  30.00   35
 51  ω     98.00 130.00   1.00    4.00    --  113.25  61.00  30.00   32
 52  ω     97.00 130.00   1.00    4.00    --  113.25  61.00 120.00   33
 53  ω     93.00 177.00   1.00    4.00    --  113.25  77.00 -60.00   84
 54  ω     83.00 109.00   1.00    4.00    --  113.25-113.00 -67.43   26
 55  ω     81.00 106.00   1.00    4.00    --  113.25 -94.00  60.00   25
 56  ω     45.00  88.00   1.00    4.00    --  113.25 -77.00  30.00   43
 57  ω     91.00 130.00   1.00    4.00    --  113.25  77.00-120.00   39
 58  ω     44.00  97.00   1.00    4.00    --  113.25 -77.00   0.00   53
 59  ω    132.00 167.00   1.00    4.00    --  113.25  77.00  60.00   35
 60  ω     43.00  69.00   1.00    4.00    --  113.25-113.00 -67.43   26
 61  ω     91.00 122.00   1.00    4.00    --  113.25  77.00  60.00   31
 62  ω    144.00 176.00   1.00    4.00    --  113.25  77.00 -90.00   32
 63  ω    141.00 177.00   1.00    4.00    --  113.25  70.00-100.54   36
 64  ω     94.00 126.00   1.00    4.00    --  113.25  77.00 -90.00   32
 65  ω     91.00 137.00   1.00    4.00    --  113.25  77.00 -15.41   46
 66  ω    150.00 177.00   1.00    4.00    --  113.25  77.00-150.00   27
 67  ω     95.00 135.00   1.00    4.00    --  113.25  70.00-100.54   40
 68  ω     91.00 117.00   1.00    4.00    --  113.25  77.00-150.00   26
 69  ω     98.00 163.00   1.00    4.00    --  113.25  61.00-150.00   65
 70  ω     97.00 159.00   1.00    4.00    --  113.25  61.00-180.00   62
 71  ω    138.00 164.00   1.00    4.00    --  113.25  61.00 -60.00   26
 72  ω     81.00 106.00   1.00    4.00    --  113.25 -94.00  90.00   25
 73  ω     98.00 134.00   1.00    4.00    --  113.25  61.00 -60.00   36
 74  ω     46.00  90.00   1.00    4.00    --  113.25 -77.00-180.00   44
 75  ω    150.00 176.00   1.00    4.00    --  113.25  77.00 150.00   26
 76  ω     42.00  68.00   1.00    4.00    --  113.25 -61.00 -90.00   26
 77  ω     93.00 140.00   1.00    4.00    --  113.25  77.00 150.00   47
 78  ω    142.00 168.00   1.00    4.00    --  113.25  77.00 120.00   26
 79  ω    137.00 165.00   1.00    4.00    --  113.25  61.00 -30.00   28
 80  ω     92.00 136.00   1.00    4.00    --  113.25  77.00 120.00   44
 81  ω    100.00 133.00   1.00    4.00    --  113.25  61.00 -30.00   33
 82  ω    109.00 135.00   1.00    4.00    --  113.25  45.00  60.00   26
 83  ω    144.00 172.00   1.00    4.00    --  113.25  45.00  60.00   28
 84  ω     79.00 105.00   1.00    4.00    --  113.25 -94.00-150.00   26
 85  ω     76.00 102.00   1.00    4.00    --  113.25 -94.00 120.00   26
 86  ω    142.00 171.00   1.00    4.00    --  113.25  77.00 -15.41   29
 87  ω     44.00  70.00   1.00    4.00    --  113.25 -94.00 120.00   26
 88  ω     42.00  68.00   1.00    4.00    --  113.25 -61.00 -60.00   26
 89  ω    136.00 162.00   1.00    4.00    --  113.25  61.00-120.00   26
 90  ω     50.00  94.00   1.00    4.00    --  113.25 -77.00-150.00   44
 91  ω     48.00  93.00   1.00    4.00    --  113.25 -77.00 -90.00   45
 92  ω     43.00  69.00   1.00    4.00    --  113.25 -94.00-150.00   26
 93  ω    131.00 176.00   1.00    4.00    --  113.25  77.00-180.00   45
 94  ω     45.00  71.00   1.00    4.00    --  113.25 -94.00 -90.00   26
 95  ω     80.00 106.00   1.00    4.00    --  113.25 -94.00 -90.00   26
 96  ω     77.00 105.00   1.00    4.00    --  113.25 -94.00   0.00   28
 97  ω     97.00 123.00   1.00    4.00    --  113.25  61.00-120.00   26
 98  ω     92.00 117.00   1.00    4.00    --  113.25  77.00-180.00   25
 99  ω     42.00  67.00   1.00    4.00    --  113.25 -61.00 150.00   25
100  ω     43.00  77.00   1.00    4.00    --  113.25 -94.00  90.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1036969
_diffrn_orient_matrix_UB_12      -0.0151851
_diffrn_orient_matrix_UB_13      0.0734103
_diffrn_orient_matrix_UB_21      -0.1061198
_diffrn_orient_matrix_UB_22      -0.0569506
_diffrn_orient_matrix_UB_23      0.0594753
_diffrn_orient_matrix_UB_31      -0.0272797
_diffrn_orient_matrix_UB_32      -0.1500485
_diffrn_orient_matrix_UB_33      -0.0880018
_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  0.0224
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51627
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.904
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.74293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.00142(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0267P)²+0.4182P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0
_reflns_number_gt                4919
_reflns_number_total             4979
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc03892d2.cif
_cod_data_source_block           21EH222_NJ-3-99
_cod_depositor_comments
'Adding full bibliography for 1572338--1572342.cif.'
_cod_database_code               1572341
_shelx_estimated_absorpt_t_min   0.565
_shelx_estimated_absorpt_t_max   0.732
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.551
_oxdiff_exptl_absorpt_empirical_full_min 0.797
_shelx_shelxl_version_number     2018/3
_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
 C18, C19A, C20A, C21A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        3. Others
 Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21C)=
 Sof(H21D)=1-FVAR(1)
 Sof(H18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H19)=Sof(H20)=
 FVAR(1)
        4.a Ternary CH refined with riding coordinates:
 C18(H18), C18(H18A), C19A(H19A)
        4.b Aromatic/amide H refined with riding coordinates:
 C20A(H20A)
        4.c X=CH2 refined with riding coordinates:
 C21(H21A,H21B), C21A(H21C,H21D)
        4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
loop_
_symmetry_equiv_pos_as_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
Zn1 Zn 0.44696(2) 0.61342(2) 0.57400(2) 0.02992(7) Uani 1 1 d . . . . .
K1 K 0.69740(3) 0.56926(3) 0.70294(2) 0.03466(8) Uani 1 1 d . . . . .
O2 O 0.54492(8) 0.57600(9) 0.44314(7) 0.03039(18) Uani 1 1 d . . . . .
O1 O 0.57616(9) 0.73697(9) 0.70930(7) 0.0357(2) Uani 1 1 d . . . . .
N2 N 0.96105(11) 0.69103(11) 0.84854(9) 0.0351(2) Uani 1 1 d . . . . .
N3 N 1.09791(12) 1.02540(12) 0.81108(10) 0.0416(3) Uani 1 1 d . . . . .
N1 N 0.72700(12) 0.49848(13) 0.89526(11) 0.0456(3) Uani 1 1 d . . . . .
C5 C 0.64362(13) 0.67756(14) 0.42213(11) 0.0379(3) Uani 1 1 d . . . . .
C1 C 0.56121(13) 0.85357(14) 0.79353(11) 0.0391(3) Uani 1 1 d . . . . .
C14 C 1.04055(15) 0.83650(15) 0.87471(12) 0.0393(3) Uani 1 1 d . . . . .
C15 C 1.01710(14) 0.87951(15) 0.78152(12) 0.0403(3) Uani 1 1 d . . . . .
C18 C 0.27270(15) 0.62614(18) 0.53730(12) 0.0491(4) Uani 1 1 d . U . . .
H18 H 0.200148 0.583889 0.57043 0.059 Uiso 0.839(6) 1 calc R U P A 1
H18A H 0.220512 0.548439 0.556078 0.059 Uiso 0.161(6) 1 calc R U P A 2
C12 C 0.95561(15) 0.67332(16) 0.95350(13) 0.0442(3) Uani 1 1 d . . . . .
C6 C 0.76535(15) 0.74551(19) 0.51451(14) 0.0509(4) Uani 1 1 d . . . . .
C11 C 0.86377(16) 0.53162(18) 0.94071(16) 0.0501(4) Uani 1 1 d . . . . .
C7 C 0.67752(16) 0.60463(18) 0.30877(13) 0.0522(4) Uani 1 1 d . . . . .
H7A H 0.710837 0.532511 0.310757 0.078 Uiso 1 1 calc R U . . .
H7B H 0.744645 0.673439 0.292528 0.078 Uiso 1 1 calc R U . . .
H7C H 0.598845 0.56112 0.250227 0.078 Uiso 1 1 calc R U . . .
C8 C 0.59132(19) 0.79015(18) 0.42049(16) 0.0531(4) Uani 1 1 d . . . . .
C17 C 1.0428(2) 1.0798(2) 0.74292(18) 0.0576(4) Uani 1 1 d . . . . .
C16 C 1.23182(17) 1.0377(2) 0.79598(16) 0.0542(4) Uani 1 1 d . . . . .
C3 C 0.44362(19) 0.8070(2) 0.84498(16) 0.0589(5) Uani 1 1 d . . . . .
C4 C 0.68560(18) 0.9295(2) 0.88324(15) 0.0602(5) Uani 1 1 d . . . . .
C13 C 1.0170(2) 0.5959(2) 0.77243(19) 0.0610(5) Uani 1 1 d . . . . .
C2 C 0.5426(2) 0.95490(18) 0.74675(17) 0.0586(4) Uani 1 1 d . . . . .
C19 C 0.2518(2) 0.7084(3) 0.48941(19) 0.0440(6) Uani 0.839(6) 1 d . . P A 1
C10 C 0.6719(2) 0.5929(2) 0.97223(18) 0.0636(5) Uani 1 1 d . . . . .
C9 C 0.6523(2) 0.3543(2) 0.8755(2) 0.0704(6) Uani 1 1 d . . . . .
C20 C 0.1272(2) 0.7278(2) 0.46940(16) 0.0489(7) Uani 0.839(6) 1 d . . P A 1
C21 C 0.1109(3) 0.8117(3) 0.4253(2) 0.0689(8) Uani 0.839(6) 1 d . . P A 1
H21A H 0.18266 0.86473 0.404104 0.083 Uiso 0.839(6) 1 calc R U P A 1
H21B H 0.027319 0.819189 0.414672 0.083 Uiso 0.839(6) 1 calc R U P A 1
H12A H 0.9289(16) 0.7499(18) 1.0059(14) 0.042(4) Uiso 1 1 d . . . . .
H15A H 0.9283(18) 0.8710(18) 0.7701(14) 0.051(5) Uiso 1 1 d . . . . .
H17A H 0.955(2) 1.0722(19) 0.7510(16) 0.057(5) Uiso 1 1 d . . . . .
H15B H 1.0319(16) 0.8171(18) 0.7116(15) 0.046(4) Uiso 1 1 d . . . . .
H14A H 1.1339(19) 0.8534(19) 0.8939(15) 0.055(5) Uiso 1 1 d . . . . .
H14B H 1.0179(16) 0.8941(18) 0.9374(15) 0.048(5) Uiso 1 1 d . . . . .
H16A H 1.235(2) 0.984(2) 0.7174(19) 0.069(6) Uiso 1 1 d . . . . .
H12B H 1.0437(18) 0.6854(19) 0.9860(15) 0.056(5) Uiso 1 1 d . . . . .
H16B H 1.281(2) 1.134(2) 0.8157(17) 0.070(6) Uiso 1 1 d . . . . .
H17B H 1.0424(19) 1.030(2) 0.6635(18) 0.062(5) Uiso 1 1 d . . . . .
H16C H 1.2740(19) 1.009(2) 0.8486(18) 0.067(6) Uiso 1 1 d . . . . .
H13B H 1.0237(19) 0.613(2) 0.7063(18) 0.062(5) Uiso 1 1 d . . . . .
H17C H 1.0932(19) 1.175(2) 0.7665(16) 0.061(5) Uiso 1 1 d . . . . .
H13A H 1.101(2) 0.614(2) 0.8125(19) 0.081(7) Uiso 1 1 d . . . . .
H13C H 0.962(2) 0.499(2) 0.7507(17) 0.068(6) Uiso 1 1 d . . . . .
H3A H 0.363(2) 0.763(2) 0.7878(18) 0.069(6) Uiso 1 1 d . . . . .
H11A H 0.8911(18) 0.459(2) 0.8911(16) 0.057(5) Uiso 1 1 d . . . . .
H2A H 0.619(2) 0.984(2) 0.7162(17) 0.064(6) Uiso 1 1 d . . . . .
H3B H 0.461(2) 0.745(2) 0.8801(19) 0.078(7) Uiso 1 1 d . . . . .
H2B H 0.463(2) 0.909(2) 0.686(2) 0.081(7) Uiso 1 1 d . . . . .
H9A H 0.691(2) 0.295(2) 0.8229(18) 0.068(6) Uiso 1 1 d . . . . .
H11B H 0.8708(18) 0.530(2) 1.0153(17) 0.063(5) Uiso 1 1 d . . . . .
H9B H 0.562(2) 0.333(2) 0.8485(17) 0.066(6) Uiso 1 1 d . . . . .
H10B H 0.674(2) 0.587(2) 1.044(2) 0.080(6) Uiso 1 1 d . . . . .
H4A H 0.761(2) 0.956(2) 0.8487(19) 0.079(7) Uiso 1 1 d . . . . .
H3C H 0.433(2) 0.886(2) 0.9046(18) 0.073(6) Uiso 1 1 d . . . . .
H9C H 0.660(2) 0.344(2) 0.9458(19) 0.076(6) Uiso 1 1 d . . . . .
H10A H 0.581(2) 0.568(2) 0.9421(18) 0.076(6) Uiso 1 1 d . . . . .
H4B H 0.679(2) 1.013(2) 0.9424(18) 0.074(6) Uiso 1 1 d . . . . .
H4C H 0.693(2) 0.862(2) 0.9131(19) 0.077(7) Uiso 1 1 d . . . . .
H2C H 0.534(2) 1.038(2) 0.805(2) 0.082(7) Uiso 1 1 d . . . . .
H10C H 0.721(2) 0.692(2) 0.9861(18) 0.078(6) Uiso 1 1 d . . . . .
H6A H 0.8014(17) 0.6765(19) 0.5120(14) 0.048(5) Uiso 1 1 d . . . . .
H6B H 0.8331(19) 0.816(2) 0.5017(16) 0.062(5) Uiso 1 1 d . . . . .
H6C H 0.7427(17) 0.7891(19) 0.5889(16) 0.054(5) Uiso 1 1 d . . . . .
H8A H 0.657(2) 0.856(2) 0.4070(17) 0.068(6) Uiso 1 1 d . . . . .
H8B H 0.511(2) 0.746(2) 0.3587(17) 0.064(5) Uiso 1 1 d . . . . .
H8C H 0.5704(19) 0.835(2) 0.4929(18) 0.062(5) Uiso 1 1 d . . . . .
H19 H 0.319(2) 0.761(2) 0.4614(18) 0.044(6) Uiso 0.839(6) 1 d . . P A 1
H20 H 0.055(2) 0.666(2) 0.4929(19) 0.058(6) Uiso 0.839(6) 1 d . . P A 1
C19A C 0.1823(12) 0.6491(14) 0.5069(8) 0.049(2) Uani 0.161(6) 1 d . U P A 2
H19A H 0.093148 0.623862 0.525762 0.059 Uiso 0.161(6) 1 calc R U P A 2
C20A C 0.2390(18) 0.7526(16) 0.4642(13) 0.065(5) Uani 0.161(6) 1 d . U P A 2
H20A H 0.331706 0.786019 0.473311 0.078 Uiso 0.161(6) 1 calc R U P A 2
C21A C 0.1765(17) 0.8057(19) 0.4143(15) 0.078(4) Uani 0.161(6) 1 d . U P A 2
H21C H 0.083634 0.776194 0.402942 0.094 Uiso 0.161(6) 1 calc R U P A 2
H21D H 0.224244 0.873516 0.389638 0.094 Uiso 0.161(6) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'
Zn Zn -1.5491 0.6778 '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 0.0937
-1 0 -1 0.1111
0 -1 -1 0.1446
1 -1 1 0.088
-1 1 -1 0.0844
0 0 1 0.0758
0 0 -1 0.111
0 -1 1 0.0761
0 1 -1 0.0463
0 1 0 0.0696
-1 -1 1 0.0795
1 0 -1 0.1121
-1 0 1 0.0724
-1 1 1 0.0925
1 -1 -1 0.1372
-1 -1 0 0.1071
1 1 0 0.0822
1 0 0 0.0807
-1 0 0 0.088
-1 -1 -1 0.1204
1 1 1 0.0779
-1 1 0 0.0875
1 -1 0 0.1188
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
Zn1 Zn1 K1 62.606(7) 2_666 2_666 ?
Zn1 Zn1 K1 63.096(7) 2_666 . ?
K1 Zn1 K1 125.702(6) . 2_666 ?
O2 Zn1 Zn1 40.54(2) . 2_666 ?
O2 Zn1 Zn1 40.52(2) 2_666 2_666 ?
O2 Zn1 K1 82.92(2) 2_666 2_666 ?
O2 Zn1 K1 83.33(2) . . ?
O2 Zn1 K1 55.14(2) 2_666 . ?
O2 Zn1 K1 54.81(2) . 2_666 ?
O2 Zn1 O2 81.06(3) . 2_666 ?
O1 Zn1 Zn1 108.38(3) . 2_666 ?
O1 Zn1 K1 48.43(3) . . ?
O1 Zn1 K1 161.40(3) . 2_666 ?
O1 Zn1 O2 100.45(4) . 2_666 ?
O1 Zn1 O2 107.34(4) . . ?
O1 Zn1 C18 125.77(5) . . ?
C18 Zn1 Zn1 125.83(4) . 2_666 ?
C18 Zn1 K1 161.37(5) . . ?
C18 Zn1 K1 65.77(4) . 2_666 ?
C18 Zn1 O2 118.74(6) . 2_666 ?
C18 Zn1 O2 114.14(5) . . ?
Zn1 K1 Zn1 54.298(7) . 2_666 ?
Zn1 K1 C13 156.47(4) . . ?
Zn1 K1 C13 116.67(4) 2_666 . ?
Zn1 K1 C10 144.65(4) 2_666 . ?
Zn1 K1 C10 114.33(4) . . ?
Zn1 K1 C19A 54.22(15) 2_666 2_666 ?
Zn1 K1 C19A 107.62(15) . 2_666 ?
O2 K1 Zn1 36.776(17) 2_666 2_666 ?
O2 K1 Zn1 36.971(18) 2_666 . ?
O2 K1 N2 173.03(3) 2_666 . ?
O2 K1 N1 115.81(3) 2_666 . ?
O2 K1 C18 69.05(3) 2_666 2_666 ?
O2 K1 C13 149.02(4) 2_666 . ?
O2 K1 C19 77.65(4) 2_666 2_666 ?
O2 K1 C10 111.72(4) 2_666 . ?
O2 K1 C19A 86.02(17) 2_666 2_666 ?
O1 K1 Zn1 86.55(2) . 2_666 ?
O1 K1 Zn1 34.284(19) . . ?
O1 K1 O2 69.46(3) . 2_666 ?
O1 K1 N2 117.50(3) . . ?
O1 K1 N1 119.82(4) . . ?
O1 K1 C18 116.72(4) . 2_666 ?
O1 K1 C13 136.81(4) . . ?
O1 K1 C19 138.38(5) . 2_666 ?
O1 K1 C10 95.55(4) . . ?
O1 K1 C19A 134.43(19) . 2_666 ?
N2 K1 Zn1 149.65(2) . . ?
N2 K1 Zn1 139.78(2) . 2_666 ?
N2 K1 C18 106.06(4) . 2_666 ?
N2 K1 C13 24.81(4) . . ?
N2 K1 C19 95.94(4) . 2_666 ?
N2 K1 C10 69.02(4) . . ?
N2 K1 C19A 88.38(17) . 2_666 ?
N1 K1 Zn1 133.12(3) . . ?
N1 K1 Zn1 135.57(3) . 2_666 ?
N1 K1 N2 61.81(3) . . ?
N1 K1 C18 120.53(4) . 2_666 ?
N1 K1 C13 69.66(5) . . ?
N1 K1 C19 96.95(5) . 2_666 ?
N1 K1 C10 24.37(4) . . ?
N1 K1 C19A 105.3(2) . 2_666 ?
C18 K1 Zn1 88.20(3) 2_666 . ?
C18 K1 Zn1 35.07(3) 2_666 2_666 ?
C18 K1 C13 81.93(4) 2_666 . ?
C18 K1 C19 23.57(6) 2_666 2_666 ?
C18 K1 C10 143.83(5) 2_666 . ?
C18 K1 C19A 19.43(16) 2_666 2_666 ?
C13 K1 C10 85.30(5) . . ?
C13 K1 C19A 63.71(16) . 2_666 ?
C19 K1 Zn1 106.15(4) 2_666 . ?
C19 K1 Zn1 52.14(4) 2_666 2_666 ?
C19 K1 C13 71.38(5) 2_666 . ?
C19 K1 C10 120.46(6) 2_666 . ?
C19 K1 C19A 15.5(2) 2_666 2_666 ?
C10 K1 C19A 129.6(2) . 2_666 ?
Zn1 O2 Zn1 98.94(3) . 2_666 ?
Zn1 O2 K1 87.89(3) 2_666 2_666 ?
Zn1 O2 K1 88.42(3) . 2_666 ?
C5 O2 Zn1 124.29(8) . 2_666 ?
C5 O2 Zn1 126.61(8) . . ?
C5 O2 K1 119.63(7) . 2_666 ?
Zn1 O1 K1 97.28(3) . . ?
C1 O1 Zn1 123.41(8) . . ?
C1 O1 K1 135.28(8) . . ?
C14 N2 K1 118.19(8) . . ?
C14 N2 C12 108.73(11) . . ?
C12 N2 K1 112.08(8) . . ?
C13 N2 K1 96.24(11) . . ?
C13 N2 C14 110.17(13) . . ?
C13 N2 C12 110.81(13) . . ?
C17 N3 C15 110.32(13) . . ?
C17 N3 C16 109.66(14) . . ?
C16 N3 C15 110.79(13) . . ?
C11 N1 K1 112.59(9) . . ?
C11 N1 C9 108.97(15) . . ?
C10 N1 K1 98.80(10) . . ?
C10 N1 C11 110.97(14) . . ?
C10 N1 C9 109.60(17) . . ?
C9 N1 K1 115.53(11) . . ?
O2 C5 C6 110.11(11) . . ?
O2 C5 C7 108.42(11) . . ?
O2 C5 C8 108.96(12) . . ?
C7 C5 C6 110.11(13) . . ?
C8 C5 C6 109.05(14) . . ?
C8 C5 C7 110.19(13) . . ?
O1 C1 C3 110.19(12) . . ?
O1 C1 C4 108.24(12) . . ?
O1 C1 C2 110.95(12) . . ?
C3 C1 C4 109.88(15) . . ?
C3 C1 C2 109.28(15) . . ?
C2 C1 C4 108.27(15) . . ?
N2 C14 C15 113.06(11) . . ?
N2 C14 H14A 110.9(10) . . ?
N2 C14 H14B 108.1(11) . . ?
C15 C14 H14A 110.1(10) . . ?
C15 C14 H14B 107.2(10) . . ?
H14A C14 H14B 107.2(14) . . ?
N3 C15 C14 111.34(12) . . ?
N3 C15 H15A 108.1(11) . . ?
N3 C15 H15B 111.1(10) . . ?
C14 C15 H15A 108.1(11) . . ?
C14 C15 H15B 110.8(10) . . ?
H15A C15 H15B 107.1(14) . . ?
Zn1 C18 K1 79.16(5) . 2_666 ?
Zn1 C18 H18 117 . . ?
Zn1 C18 H18A 96 . . ?
K1 C18 H18 117 2_666 . ?
K1 C18 H18A 96 2_666 . ?
C19 C18 Zn1 124.78(16) . . ?
C19 C18 K1 86.48(12) . 2_666 ?
C19 C18 H18 117 . . ?
C19A C18 Zn1 167.7(8) . . ?
C19A C18 H18A 96 . . ?
N2 C12 C11 114.60(13) . . ?
N2 C12 H12A 106.9(9) . . ?
N2 C12 H12B 108.7(11) . . ?
C11 C12 H12A 110.4(9) . . ?
C11 C12 H12B 107.6(11) . . ?
H12A C12 H12B 108.5(14) . . ?
C5 C6 H6A 109.0(11) . . ?
C5 C6 H6B 110.9(11) . . ?
C5 C6 H6C 110.3(10) . . ?
H6A C6 H6B 105.9(15) . . ?
H6A C6 H6C 111.1(15) . . ?
H6B C6 H6C 109.5(15) . . ?
N1 C11 C12 114.54(12) . . ?
N1 C11 H11A 107.0(11) . . ?
N1 C11 H11B 109.6(11) . . ?
C12 C11 H11A 109.6(11) . . ?
C12 C11 H11B 107.4(11) . . ?
H11A C11 H11B 108.6(16) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 108.2(12) . . ?
C5 C8 H8B 109.7(11) . . ?
C5 C8 H8C 109.1(11) . . ?
H8A C8 H8B 109.6(16) . . ?
H8A C8 H8C 109.0(17) . . ?
H8B C8 H8C 111.1(16) . . ?
N3 C17 H17A 111.1(11) . . ?
N3 C17 H17B 112.2(12) . . ?
N3 C17 H17C 108.8(12) . . ?
H17A C17 H17B 107.7(16) . . ?
H17A C17 H17C 108.3(16) . . ?
H17B C17 H17C 108.6(17) . . ?
N3 C16 H16A 111.7(12) . . ?
N3 C16 H16B 108.1(13) . . ?
N3 C16 H16C 110.3(12) . . ?
H16A C16 H16B 107.8(17) . . ?
H16A C16 H16C 111.9(17) . . ?
H16B C16 H16C 106.9(17) . . ?
C1 C3 H3A 109.7(12) . . ?
C1 C3 H3B 108.0(13) . . ?
C1 C3 H3C 111.6(13) . . ?
H3A C3 H3B 114.6(18) . . ?
H3A C3 H3C 106.2(17) . . ?
H3B C3 H3C 106.7(17) . . ?
C1 C4 H4A 109.3(13) . . ?
C1 C4 H4B 110.3(12) . . ?
C1 C4 H4C 106.1(13) . . ?
H4A C4 H4B 110.4(18) . . ?
H4A C4 H4C 109.8(18) . . ?
H4B C4 H4C 111.0(18) . . ?
N2 C13 H13B 108.9(12) . . ?
N2 C13 H13A 106.8(14) . . ?
N2 C13 H13C 110.6(12) . . ?
H13B C13 H13A 112.1(18) . . ?
H13B C13 H13C 108.9(17) . . ?
H13A C13 H13C 109.5(18) . . ?
C1 C2 H2A 107.2(12) . . ?
C1 C2 H2B 111.5(13) . . ?
C1 C2 H2C 111.9(13) . . ?
H2A C2 H2B 109.2(17) . . ?
H2A C2 H2C 109.0(18) . . ?
H2B C2 H2C 108.1(18) . . ?
K1 C19 H19 83.6(13) 2_666 . ?
C18 C19 K1 69.94(11) . 2_666 ?
C18 C19 C20 125.9(2) . . ?
C18 C19 H19 123.4(15) . . ?
C20 C19 K1 118.06(13) . 2_666 ?
C20 C19 H19 110.7(15) . . ?
N1 C10 H10B 112.1(13) . . ?
N1 C10 H10A 109.9(13) . . ?
N1 C10 H10C 110.6(13) . . ?
H10B C10 H10A 106.3(18) . . ?
H10B C10 H10C 107.9(18) . . ?
H10A C10 H10C 109.9(18) . . ?
N1 C9 H9A 106.8(13) . . ?
N1 C9 H9B 109.2(12) . . ?
N1 C9 H9C 109.3(13) . . ?
H9A C9 H9B 113.1(18) . . ?
H9A C9 H9C 109.2(18) . . ?
H9B C9 H9C 109.1(17) . . ?
C19 C20 H20 110.8(13) . . ?
C21 C20 C19 124.4(3) . . ?
C21 C20 H20 124.8(13) . . ?
C20 C21 H21A 120 . . ?
C20 C21 H21B 120 . . ?
H21A C21 H21B 120 . . ?
K1 C19A H19A 127 2_666 . ?
C18 C19A K1 63.6(4) . 2_666 ?
C18 C19A H19A 127 . . ?
C18 C19A C20A 104.1(13) . . ?
C20A C19A H19A 127 . . ?
C19A C20A H20A 116.3 . . ?
C21A C20A C19A 127.4(16) . . ?
C21A C20A H20A 116.3 . . ?
C20A C21A H21C 120 . . ?
C20A C21A H21D 120 . . ?
H21C C21A H21D 120 . . ?
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
Zn1 Zn1 3.1124(3) 2_666 ?
Zn1 K1 3.4179(3) 2_666 ?
Zn1 K1 3.4030(3) . ?
Zn1 O2 2.0480(9) 2_666 ?
Zn1 O2 2.0470(8) . ?
Zn1 O1 1.9325(9) . ?
Zn1 C18 1.9998(15) . ?
K1 O2 2.7942(9) 2_666 ?
K1 O1 2.5667(9) . ?
K1 N2 2.9796(11) . ?
K1 N1 2.9492(12) . ?
K1 C18 3.1735(15) 2_666 ?
K1 C13 3.457(2) . ?
K1 C19 3.372(2) 2_666 ?
K1 C10 3.482(2) . ?
K1 C19A 3.518(10) 2_666 ?
O2 C5 1.4231(15) . ?
O1 C1 1.4033(15) . ?
N2 C14 1.4661(17) . ?
N2 C12 1.4679(18) . ?
N2 C13 1.459(2) . ?
N3 C15 1.4646(18) . ?
N3 C17 1.451(2) . ?
N3 C16 1.458(2) . ?
N1 C11 1.460(2) . ?
N1 C10 1.454(2) . ?
N1 C9 1.463(2) . ?
C5 C6 1.529(2) . ?
C5 C7 1.526(2) . ?
C5 C8 1.526(2) . ?
C1 C3 1.524(2) . ?
C1 C4 1.526(2) . ?
C1 C2 1.525(2) . ?
C14 C15 1.511(2) . ?
C14 H14A 0.980(19) . ?
C14 H14B 0.929(18) . ?
C15 H15A 0.945(18) . ?
C15 H15B 0.972(18) . ?
C18 H18 1 . ?
C18 H18A 1 . ?
C18 C19 1.351(3) . ?
C18 C19A 1.179(10) . ?
C12 C11 1.519(2) . ?
C12 H12A 1.001(17) . ?
C12 H12B 0.981(19) . ?
C6 H6A 0.950(18) . ?
C6 H6B 0.97(2) . ?
C6 H6C 0.994(19) . ?
C11 H11A 0.96(2) . ?
C11 H11B 0.99(2) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 H8A 0.93(2) . ?
C8 H8B 1.01(2) . ?
C8 H8C 0.97(2) . ?
C17 H17A 0.95(2) . ?
C17 H17B 0.98(2) . ?
C17 H17C 0.94(2) . ?
C16 H16A 0.98(2) . ?
C16 H16B 0.95(2) . ?
C16 H16C 1.00(2) . ?
C3 H3A 0.99(2) . ?
C3 H3B 1.01(2) . ?
C3 H3C 0.97(2) . ?
C4 H4A 0.98(2) . ?
C4 H4B 0.98(2) . ?
C4 H4C 0.99(2) . ?
C13 H13B 0.96(2) . ?
C13 H13A 0.96(2) . ?
C13 H13C 0.97(2) . ?
C2 H2A 0.96(2) . ?
C2 H2B 1.00(2) . ?
C2 H2C 0.98(2) . ?
C19 C20 1.467(3) . ?
C19 H19 0.97(2) . ?
C10 H10B 0.97(2) . ?
C10 H10A 0.96(2) . ?
C10 H10C 1.00(2) . ?
C9 H9A 0.97(2) . ?
C9 H9B 0.95(2) . ?
C9 H9C 0.98(2) . ?
C20 C21 1.315(3) . ?
C20 H20 1.03(2) . ?
C21 H21A 0.95 . ?
C21 H21B 0.95 . ?
C19A H19A 1 . ?
C19A C20A 1.45(2) . ?
C20A H20A 0.95 . ?
C20A C21A 1.32(2) . ?
C21A H21C 0.95 . ?
C21A H21D 0.95 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C6 H6C O1 0.994(19) 2.548(19) 3.383(2) 141.4(14) . yes
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
Zn1 O2 C5 C6 -71.88(14) 2_666 . . . ?
Zn1 O2 C5 C6 65.94(15) . . . . ?
Zn1 O2 C5 C7 48.64(14) 2_666 . . . ?
Zn1 O2 C5 C7 -173.55(9) . . . . ?
Zn1 O2 C5 C8 -53.62(14) . . . . ?
Zn1 O2 C5 C8 168.57(9) 2_666 . . . ?
Zn1 O1 C1 C3 62.96(16) . . . . ?
Zn1 O1 C1 C4 -176.87(12) . . . . ?
Zn1 O1 C1 C2 -58.21(16) . . . . ?
Zn1 C18 C19 K1 74.21(11) . . . 2_666 ?
Zn1 C18 C19 C20 -175.07(15) . . . . ?
Zn1 C18 C19A K1 71(2) . . . 2_666 ?
Zn1 C18 C19A C20A -6(3) . . . . ?
K1 O2 C5 C6 178.46(10) 2_666 . . . ?
K1 O2 C5 C7 -61.03(13) 2_666 . . . ?
K1 O2 C5 C8 58.90(13) 2_666 . . . ?
K1 O1 C1 C3 -88.92(15) . . . . ?
K1 O1 C1 C4 31.25(19) . . . . ?
K1 O1 C1 C2 149.91(11) . . . . ?
K1 N2 C14 C15 -31.67(16) . . . . ?
K1 N2 C12 C11 40.92(16) . . . . ?
K1 N1 C11 C12 44.18(18) . . . . ?
K1 C18 C19 C20 110.7(2) 2_666 . . . ?
K1 C18 C19A C20A -77.5(8) 2_666 . . . ?
K1 C19 C20 C21 -97.3(3) 2_666 . . . ?
K1 C19A C20A C21A 114.2(16) 2_666 . . . ?
N2 C14 C15 N3 179.81(12) . . . . ?
N2 C12 C11 N1 -60.2(2) . . . . ?
C14 N2 C12 C11 173.45(13) . . . . ?
C18 C19 C20 C21 178.1(2) . . . . ?
C18 C19A C20A C21A 175.4(15) . . . . ?
C12 N2 C14 C15 -160.89(13) . . . . ?
C17 N3 C15 C14 -159.36(15) . . . . ?
C16 N3 C15 C14 79.01(16) . . . . ?
C13 N2 C14 C15 77.49(17) . . . . ?
C13 N2 C12 C11 -65.32(18) . . . . ?
C10 N1 C11 C12 -65.51(19) . . . . ?
C9 N1 C11 C12 173.72(17) . . . . ?
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
1.0003 -0.0001 0.9997 0.1771 -0.0467 -0.1152
-1.0003 0.0001 -0.9997 -0.1771 0.0467 0.1152
-0.0003 -1.0001 -0.9999 -0.0582 -0.0025 0.2381
1.0002 -1.0003 0.9997 0.1923 0.0103 0.0348
-1.0002 1.0003 -0.9997 -0.1923 -0.0103 -0.0348
0.0002 -0.0001 0.9999 0.0734 0.0594 -0.088
-0.0002 0.0001 -0.9999 -0.0734 -0.0594 0.088
0.0002 -1.0003 1 0.0886 0.1164 0.0621
-0.0002 1.0003 -1 -0.0886 -0.1164 -0.0621
0 1.0002 -0.0001 -0.0152 -0.057 -0.1501
-0.9998 -1.0003 1.0003 -0.0151 0.2226 0.0893
0.9998 0.0001 -1.0002 0.0302 -0.1656 0.0607
-0.9998 -0.0001 1.0002 -0.0302 0.1656 -0.0607
-0.9997 1.0001 1.0002 -0.0454 0.1086 -0.2108
0.9997 -1.0001 -1.0002 0.0454 -0.1086 0.2108
-1.0001 -1.0002 0.0003 -0.0885 0.1631 0.1773
1.0001 1.0002 -0.0003 0.0885 -0.1631 -0.1773
1 0 -0.0003 0.1037 -0.1061 -0.0273
-1 0 0.0003 -0.1037 0.1061 0.0273
-1.0003 -1.0001 -0.9996 -0.1619 0.1037 0.2653
1.0003 1.0001 0.9996 0.1619 -0.1037 -0.2653
-1 1.0002 0.0002 -0.1189 0.0492 -0.1228
1 -1.0002 -0.0002 0.1189 -0.0492 0.1228
