#------------------------------------------------------------------------------
#$Date: 2024-10-06 09:00:42 +0200 (Sun 06 de Oct de 2024) $
#$Revision: 295180 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/23/1572339.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_1572339
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         'C52 H82 K2 O8 Zn2'
_chemical_formula_sum            'C52 H82 K2 O8 Zn2'
_chemical_formula_weight         1044.11
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-23T19:00:21-00:00
_audit_update_record
;
2024-05-26 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.7772(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2697(3)
_cell_length_b                   17.0018(3)
_cell_length_c                   20.8902(3)
_cell_measurement_reflns_used    24674
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      76.88
_cell_measurement_theta_min      3.451
_cell_volume                     5982.85(19)
_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  (Sheldrick, 2015)'
_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 1
_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    -97.00  -9.00   0.50    3.00    --  -23.00 -16.00  36.00  176
  2  ω    -28.00  52.00   0.50    3.00    --  -23.00  16.00-153.00  160
  3  ω     35.00 122.00   0.50    3.00    --   47.92  16.00-153.00  174
  4  ω    -26.00  22.00   0.50    3.00    --   47.92 -16.00  36.00   96
  5  ω    100.00 177.00   0.50   21.00    --  113.25  16.00-153.00  154
  6  ω    -30.00  53.00   0.50    3.00    --  -23.00  19.00 -60.00  166
  7  ω    -36.00  49.00   0.50    3.00    --  -23.00  45.00  90.00  170
  8  ω     -1.00  81.00   0.50    3.00    --   47.92 -99.00 -60.00  164
  9  ω    -26.00  23.00   0.50    3.00    --   47.92 -19.00-180.00   98
 10  ω     -1.00  81.00   0.50    3.00    --   47.92 -99.00-150.00  164
 11  ω     -1.00  81.00   0.50    3.00    --   47.92 -99.00  30.00  164
 12  ω    -26.00  23.00   0.50    3.00    --   47.92 -19.00 -90.00   98
 13  ω    -26.00  23.00   0.50    3.00    --   47.92 -19.00-120.00   98
 14  ω    -23.00  63.00   0.50    3.00    --   47.92 -57.00   0.00  172
 15  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00-120.00  128
 16  ω    101.00 177.00   0.50   21.00    --  113.25  30.00   0.00  152
 17  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00 120.00  128
 18  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00  30.00  128
 19  ω    100.00 177.00   0.50   21.00    --  113.25  15.00 -90.00  154
 20  ω     91.00 177.00   0.50   21.00    --  113.25  77.00 120.00  172
 21  ω     42.00 102.00   0.50   21.00    --  113.25 -77.00 -60.00  120
 22  ω     42.00 102.00   0.50   21.00    --  113.25 -77.00 -90.00  120
 23  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00  60.00  128
 24  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00-180.00  128
 25  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00 -30.00  128
 26  ω     42.00 102.00   0.50   21.00    --  113.25 -77.00-120.00  120
 27  ω    101.00 177.00   0.50   21.00    --  113.25  30.00 120.00  152
 28  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00-150.00  128
 29  ω    101.00 177.00   0.50   21.00    --  113.25  45.00  30.00  152
 30  ω     42.00  68.00   0.50   21.00    --  113.25 -61.00 120.00   52
 31  ω     91.00 177.00   0.50   21.00    --  113.25  77.00  30.00  172
 32  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00   0.00  128
 33  ω     42.00 102.00   0.50   21.00    --  113.25 -77.00  30.00  120
 34  ω     42.00 102.00   0.50   21.00    --  113.25 -77.00 120.00  120
 35  ω     42.00  68.00   0.50   21.00    --  113.25 -61.00 150.00   52
 36  ω     42.00  68.00   0.50   21.00    --  113.25 -61.00  30.00   52
 37  ω    101.00 177.00   0.50   21.00    --  113.25  45.00  90.00  152
 38  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00 150.00  128
 39  ω     42.00  68.00   0.50   21.00    --  113.25 -61.00-150.00   52
 40  ω     42.00 102.00   0.50   21.00    --  113.25 -77.00 -30.00  120
 41  ω     42.00  68.00   0.50   21.00    --  113.25 -61.00-180.00   52
 42  ω     42.00 106.00   0.50   21.00    --  113.25-100.00 108.96  128
 43  ω     42.00  68.00   0.50   21.00    --  113.25 -61.00  60.00   52
 44  ω     42.00 106.00   0.50   21.00    --  113.25 -94.00 -90.00  128
 45  ω    101.00 177.00   0.50   21.00    --  113.25  30.00 -30.00  152
 46  ω    101.00 177.00   0.50   21.00    --  113.25  45.00 -90.00  152
 47  ω     42.00 108.00   0.50   21.00    --  113.25-111.00-147.12  132
 48  ω     25.00 121.00   0.50    3.00    --   47.92  77.00   0.00  192
 49  ω     25.00 121.00   0.50    3.00    --   47.92  77.00 -90.00  192
;
_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      -0.0594015
_diffrn_orient_matrix_UB_12      0.0674234
_diffrn_orient_matrix_UB_13      -0.0089082
_diffrn_orient_matrix_UB_21      0.0675161
_diffrn_orient_matrix_UB_22      0.0603814
_diffrn_orient_matrix_UB_23      0.0148706
_diffrn_orient_matrix_UB_31      -0.0166768
_diffrn_orient_matrix_UB_32      0.0037036
_diffrn_orient_matrix_UB_33      -0.078115
_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  0.0602
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59420
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.265
_diffrn_reflns_theta_min         3.467
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5794
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1303P)²+4.8608P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1977
_refine_ls_wR_factor_ref         0.2066
_reflns_Friedel_coverage         0
_reflns_number_gt                4850
_reflns_number_total             5794
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc03892d2.cif
_cod_data_source_block           22EH021_NJ-3-118
_cod_depositor_comments
'Adding full bibliography for 1572338--1572342.cif.'
_cod_original_cell_volume        5982.84(18)
_cod_database_code               1572339
_shelx_estimated_absorpt_t_min   0.729
_shelx_estimated_absorpt_t_max   0.846
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.599
_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. Restrained distances
 C22-C21 = C20-C19
 1.53 with sigma of 0.02
 C24-C25
 1.54 with sigma of 0.001
 O3-C22 = O3-C19
 1.44 with sigma of 0.02
 C25-C26 = C23-C24
 1.53 with sigma of 0.001
 C21-C20
 1.54 with sigma of 0.001
 O3-C21 = O3-C20 = C22-C20 = C21-C19
 2.38 with sigma of 0.04
 O4-C26 \\sim O4-C23
 with sigma of 0.002
 O3-C22 \\sim O3-C19
 with sigma of 0.02
 C22-C21 \\sim C21-C20 \\sim C20-C19
 with sigma of 0.02
 C21-C19 \\sim C22-C20
 with sigma of 0.04
 O3-C21 \\sim O3-C20
 with sigma of 0.04
        3. Uiso/Uaniso restraints and constraints
O3 \\sim C22 \\sim C21 \\sim C20 \\sim C19: within 2A with sigma of 0.04 and
        sigma for terminal atoms of 0.08 within 2A
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.02 and sigma for
        terminal atoms of 0.01
        4. Rigid body (RIGU) restrains
 O3, C22, C21, C20, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
        5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C22(H22A,
 H22B), C21(H21A,H21B), C20(H20A,H20B), C19(H19A,H19B)
        5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C11(H11), C10(H10), C16(H16), C13(H13), C15(H15), C14(H14)
        5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C2(H2A,
 H2B,H2C), C4(H4A,H4B,H4C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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 0.32098(2) 0.68944(3) 0.77967(2) 0.0649(2) Uani 1 1 d . . . . .
K1 K 0.36384(5) 0.87256(6) 0.73890(4) 0.0804(3) Uani 1 1 d . . . . .
O2 O 0.25496(13) 0.74732(14) 0.68925(9) 0.0630(5) Uani 1 1 d . . . . .
O1 O 0.41881(15) 0.74793(19) 0.80721(13) 0.0839(7) Uani 1 1 d . . . . .
O4 O 0.4080(2) 0.8952(2) 0.63022(18) 0.1092(11) Uani 1 1 d D . . . .
C9 C 0.3144(2) 0.5711(2) 0.78828(17) 0.0710(8) Uani 1 1 d . . . . .
C17 C 0.2957(2) 0.4520(2) 0.84871(18) 0.0760(9) Uani 1 1 d . . . . .
C12 C 0.3108(3) 0.4013(3) 0.8011(2) 0.0817(10) Uani 1 1 d . . . . .
C18 C 0.2980(2) 0.5345(2) 0.83998(17) 0.0727(8) Uani 1 1 d . . . . .
H18 H 0.28742 0.567119 0.872332 0.087 Uiso 1 1 calc R U . . .
C11 C 0.3299(3) 0.4375(3) 0.7483(2) 0.0908(12) Uani 1 1 d . . . . .
H11 H 0.342061 0.405642 0.716353 0.109 Uiso 1 1 calc R U . . .
C10 C 0.3310(3) 0.5173(3) 0.7429(2) 0.0838(11) Uani 1 1 d . . . . .
H10 H 0.343742 0.538717 0.706442 0.101 Uiso 1 1 calc R U . . .
C5 C 0.2370(2) 0.7164(2) 0.62173(15) 0.0676(8) Uani 1 1 d . . . . .
C7 C 0.1988(3) 0.7800(3) 0.56769(16) 0.0798(10) Uani 1 1 d . . . . .
H7A H 0.153369 0.802584 0.575161 0.12 Uiso 1 1 calc R U . . .
H7B H 0.180696 0.756985 0.521121 0.12 Uiso 1 1 calc R U . . .
H7C H 0.237744 0.821457 0.572047 0.12 Uiso 1 1 calc R U . . .
C16 C 0.2793(3) 0.4159(3) 0.9031(2) 0.0873(11) Uani 1 1 d . . . . .
H16 H 0.26851 0.448216 0.935454 0.105 Uiso 1 1 calc R U . . .
C6 C 0.1799(3) 0.6464(3) 0.60868(19) 0.0842(10) Uani 1 1 d . . . . .
H6A H 0.202648 0.607331 0.645585 0.126 Uiso 1 1 calc R U . . .
H6B H 0.171641 0.622477 0.563731 0.126 Uiso 1 1 calc R U . . .
H6C H 0.128907 0.664749 0.608403 0.126 Uiso 1 1 calc R U . . .
C8 C 0.3147(3) 0.6898(2) 0.61639(19) 0.0789(10) Uani 1 1 d . . . . .
H8A H 0.348011 0.735777 0.618809 0.118 Uiso 1 1 calc R U . . .
H8B H 0.30277 0.662522 0.572134 0.118 Uiso 1 1 calc R U . . .
H8C H 0.343029 0.653972 0.654803 0.118 Uiso 1 1 calc R U . . .
C13 C 0.3100(3) 0.3192(3) 0.8100(3) 0.0994(13) Uani 1 1 d . . . . .
H13 H 0.321771 0.285465 0.779014 0.119 Uiso 1 1 calc R U . . .
C15 C 0.2785(3) 0.3368(3) 0.9100(3) 0.1039(14) Uani 1 1 d . . . . .
H15 H 0.268413 0.314432 0.947426 0.125 Uiso 1 1 calc R U . . .
C1 C 0.4971(2) 0.7206(4) 0.8398(2) 0.0977(13) Uani 1 1 d . . . . .
C14 C 0.2928(4) 0.2876(3) 0.8618(3) 0.1097(15) Uani 1 1 d . . . . .
H14 H 0.290217 0.232108 0.865804 0.132 Uiso 1 1 calc R U . . .
C23 C 0.3778(4) 0.9521(4) 0.5777(4) 0.132(2) Uani 1 1 d D . . . .
H23A H 0.368872 1.002177 0.597775 0.158 Uiso 1 1 calc R U . . .
H23B H 0.326423 0.934228 0.542493 0.158 Uiso 1 1 calc R U . . .
C3 C 0.5136(4) 0.6951(5) 0.9112(3) 0.144(3) Uani 1 1 d . U . . .
H3A H 0.516896 0.741249 0.940348 0.216 Uiso 1 1 calc R U . . .
H3B H 0.564168 0.666575 0.929482 0.216 Uiso 1 1 calc R U . . .
H3C H 0.470885 0.660516 0.911546 0.216 Uiso 1 1 calc R U . . .
C24 C 0.4376(5) 0.9646(5) 0.5438(5) 0.186(4) Uani 1 1 d D . . . .
H24A H 0.467567 1.014152 0.560106 0.223 Uiso 1 1 calc R U . . .
H24B H 0.410646 0.966206 0.492601 0.223 Uiso 1 1 calc R U . . .
C2 C 0.5522(3) 0.7805(5) 0.8341(5) 0.163(3) Uani 1 1 d . U . . .
H2A H 0.535424 0.797024 0.785529 0.245 Uiso 1 1 calc R U . . .
H2B H 0.605877 0.758333 0.849999 0.245 Uiso 1 1 calc R U . . .
H2C H 0.552165 0.825976 0.86283 0.245 Uiso 1 1 calc R U . . .
C4 C 0.5118(4) 0.6531(6) 0.7990(4) 0.163(3) Uani 1 1 d . U . . .
H4A H 0.476819 0.609052 0.798109 0.245 Uiso 1 1 calc R U . . .
H4B H 0.567277 0.636215 0.821023 0.245 Uiso 1 1 calc R U . . .
H4C H 0.500775 0.670307 0.751356 0.245 Uiso 1 1 calc R U . . .
C25 C 0.4926(4) 0.8927(5) 0.5676(4) 0.157(3) Uani 1 1 d D U . . .
H25A H 0.481466 0.854702 0.529052 0.189 Uiso 1 1 calc R U . . .
H25B H 0.548997 0.908895 0.584016 0.189 Uiso 1 1 calc R U . . .
C26 C 0.4744(4) 0.8566(4) 0.6267(4) 0.151(3) Uani 1 1 d D U . . .
H26A H 0.463172 0.799753 0.61822 0.182 Uiso 1 1 calc R U . . .
H26B H 0.520629 0.862839 0.671201 0.182 Uiso 1 1 calc R U . . .
O3 O 0.4300(3) 1.0006(3) 0.8192(3) 0.1386(14) Uani 1 1 d D U . . .
C22 C 0.3871(5) 1.0668(5) 0.8206(5) 0.165(3) Uani 1 1 d D U . . .
H22A H 0.340213 1.051533 0.830449 0.198 Uiso 1 1 calc R U . . .
H22B H 0.367995 1.092887 0.774637 0.198 Uiso 1 1 calc R U . . .
C21 C 0.4364(6) 1.1217(6) 0.8740(6) 0.222(5) Uani 1 1 d D U . . .
H21A H 0.408599 1.139917 0.903595 0.266 Uiso 1 1 calc R U . . .
H21B H 0.451481 1.167901 0.852937 0.266 Uiso 1 1 calc R U . . .
C20 C 0.5096(6) 1.0717(6) 0.9158(5) 0.206(4) Uani 1 1 d D U . . .
H20A H 0.559299 1.101752 0.926299 0.247 Uiso 1 1 calc R U . . .
H20B H 0.50709 1.053198 0.95989 0.247 Uiso 1 1 calc R U . . .
C19 C 0.5042(5) 1.0059(6) 0.8691(6) 0.219(5) Uani 1 1 d D U . . .
H19A H 0.542953 1.01342 0.847195 0.262 Uiso 1 1 calc R U . . .
H19B H 0.517498 0.95631 0.896053 0.262 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 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'
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 1 -1 0.0425
-1 1 0 0.0355
1 -1 0 0.0337
-1 1 1 0.0429
1 -1 -1 0.0264
0 -1 1 0.0314
0 -1 -1 0.0461
1 1 -1 0.0364
-1 -1 1 0.0364
-1 -1 0 0.0298
1 1 0 0.0371
1 1 1 0.0348
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
K1 Zn1 K1 124.630(18) . 7_566 ?
O2 Zn1 K1 80.84(6) . 7_566 ?
O2 Zn1 K1 81.30(7) 7_566 . ?
O2 Zn1 K1 55.72(7) 7_566 7_566 ?
O2 Zn1 K1 56.04(7) . . ?
O2 Zn1 O2 79.14(8) 7_566 . ?
O1 Zn1 K1 47.58(8) . . ?
O1 Zn1 K1 162.77(9) . 7_566 ?
O1 Zn1 O2 99.99(10) . . ?
O1 Zn1 O2 107.33(11) . 7_566 ?
O1 Zn1 C9 124.41(13) . . ?
C9 Zn1 K1 67.27(10) . 7_566 ?
C9 Zn1 K1 163.46(10) . . ?
C9 Zn1 O2 121.50(12) . . ?
C9 Zn1 O2 114.95(12) . 7_566 ?
Zn1 K1 Zn1 55.371(18) . 7_566 ?
O2 K1 Zn1 37.16(4) . . ?
O2 K1 Zn1 36.86(4) . 7_566 ?
O2 K1 C9 68.89(9) . 7_566 ?
O2 K1 C18 78.66(9) . 7_566 ?
O1 K1 Zn1 34.16(6) . . ?
O1 K1 Zn1 87.98(6) . 7_566 ?
O1 K1 O2 69.24(8) . . ?
O1 K1 O4 114.08(10) . . ?
O1 K1 C9 120.01(9) . 7_566 ?
O1 K1 C18 142.23(10) . 7_566 ?
O1 K1 O3 109.66(13) . . ?
O4 K1 Zn1 120.74(9) . . ?
O4 K1 Zn1 123.35(9) . 7_566 ?
O4 K1 O2 101.23(10) . . ?
O4 K1 C9 114.65(9) . 7_566 ?
O4 K1 C18 90.80(9) . 7_566 ?
O4 K1 O3 101.35(15) . . ?
C9 K1 Zn1 35.43(7) 7_566 7_566 ?
C9 K1 Zn1 90.08(7) 7_566 . ?
C18 K1 Zn1 54.26(7) 7_566 7_566 ?
C18 K1 Zn1 109.00(8) 7_566 . ?
C18 K1 C9 24.74(9) 7_566 7_566 ?
O3 K1 Zn1 119.97(11) . 7_566 ?
O3 K1 Zn1 131.85(11) . . ?
O3 K1 O2 155.39(12) . . ?
O3 K1 C9 92.73(13) . 7_566 ?
O3 K1 C18 91.36(13) . 7_566 ?
Zn1 O2 Zn1 100.86(8) 7_566 . ?
Zn1 O2 K1 87.42(8) 7_566 . ?
Zn1 O2 K1 86.80(8) . . ?
C5 O2 Zn1 124.3(2) . . ?
C5 O2 Zn1 125.78(19) . 7_566 ?
C5 O2 K1 120.20(19) . . ?
Zn1 O1 K1 98.26(10) . . ?
C1 O1 Zn1 128.8(3) . . ?
C1 O1 K1 131.0(3) . . ?
C23 O4 K1 126.6(3) . . ?
C26 O4 K1 121.3(3) . . ?
C26 O4 C23 111.5(4) . . ?
Zn1 C9 K1 77.30(10) . 7_566 ?
C18 C9 Zn1 123.8(3) . . ?
C18 C9 K1 76.2(2) . 7_566 ?
C18 C9 C10 113.5(4) . . ?
C10 C9 Zn1 122.7(3) . . ?
C10 C9 K1 122.1(3) . 7_566 ?
C12 C17 C16 117.1(4) . . ?
C18 C17 C12 119.1(3) . . ?
C18 C17 C16 123.8(4) . . ?
C11 C12 C17 117.0(4) . . ?
C13 C12 C17 119.6(4) . . ?
C13 C12 C11 123.3(4) . . ?
K1 C18 H18 71 7_566 . ?
C9 C18 K1 79.1(2) . 7_566 ?
C9 C18 C17 125.0(3) . . ?
C9 C18 H18 117.5 . . ?
C17 C18 K1 119.3(3) . 7_566 ?
C17 C18 H18 117.5 . . ?
C12 C11 H11 119.6 . . ?
C10 C11 C12 120.8(4) . . ?
C10 C11 H11 119.6 . . ?
C9 C10 H10 117.7 . . ?
C11 C10 C9 124.5(4) . . ?
C11 C10 H10 117.7 . . ?
O2 C5 C7 109.7(3) . . ?
O2 C5 C6 110.0(3) . . ?
O2 C5 C8 108.5(3) . . ?
C7 C5 C6 109.5(3) . . ?
C7 C5 C8 109.1(3) . . ?
C8 C5 C6 110.0(3) . . ?
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 . . ?
C17 C16 H16 119 . . ?
C15 C16 C17 121.9(4) . . ?
C15 C16 H16 119 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.1(5) . . ?
C14 C13 H13 119.4 . . ?
C16 C15 H15 119.9 . . ?
C16 C15 C14 120.1(5) . . ?
C14 C15 H15 119.9 . . ?
O1 C1 C3 111.1(4) . . ?
O1 C1 C2 109.5(4) . . ?
O1 C1 C4 110.3(5) . . ?
C3 C1 C4 109.7(6) . . ?
C2 C1 C3 114.2(6) . . ?
C2 C1 C4 101.7(6) . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
O4 C23 H23A 109.9 . . ?
O4 C23 H23B 109.9 . . ?
O4 C23 C24 108.8(4) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C23 C24 H24A 111 . . ?
C23 C24 H24B 111 . . ?
C23 C24 C25 103.6(5) . . ?
H24A C24 H24B 109 . . ?
C25 C24 H24A 111 . . ?
C25 C24 H24B 111 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C24 C25 H25A 110.7 . . ?
C24 C25 H25B 110.7 . . ?
H25A C25 H25B 108.8 . . ?
C26 C25 C24 105.1(5) . . ?
C26 C25 H25A 110.7 . . ?
C26 C25 H25B 110.7 . . ?
O4 C26 C25 108.5(4) . . ?
O4 C26 H26A 110 . . ?
O4 C26 H26B 110 . . ?
C25 C26 H26A 110 . . ?
C25 C26 H26B 110 . . ?
H26A C26 H26B 108.4 . . ?
C22 O3 K1 123.0(4) . . ?
C19 O3 K1 126.8(5) . . ?
C19 O3 C22 109.7(6) . . ?
O3 C22 H22A 109.6 . . ?
O3 C22 H22B 109.6 . . ?
O3 C22 C21 110.4(6) . . ?
H22A C22 H22B 108.1 . . ?
C21 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C22 C21 H21A 111.2 . . ?
C22 C21 H21B 111.2 . . ?
C22 C21 C20 102.9(6) . . ?
H21A C21 H21B 109.1 . . ?
C20 C21 H21A 111.2 . . ?
C20 C21 H21B 111.2 . . ?
C21 C20 H20A 111.2 . . ?
C21 C20 H20B 111.2 . . ?
H20A C20 H20B 109.1 . . ?
C19 C20 C21 102.9(6) . . ?
C19 C20 H20A 111.2 . . ?
C19 C20 H20B 111.2 . . ?
O3 C19 C20 110.7(7) . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
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 K1 3.3983(10) . ?
Zn1 K1 3.4130(10) 7_566 ?
Zn1 O2 2.049(2) 7_566 ?
Zn1 O2 2.056(2) . ?
Zn1 O1 1.928(3) . ?
Zn1 C9 2.028(4) . ?
K1 O2 2.823(3) . ?
K1 O1 2.535(3) . ?
K1 O4 2.715(3) . ?
K1 C9 3.227(4) 7_566 ?
K1 C18 3.191(4) 7_566 ?
K1 O3 2.728(5) . ?
O2 C5 1.420(4) . ?
O1 C1 1.404(5) . ?
O4 C23 1.406(5) . ?
O4 C26 1.406(5) . ?
C9 C18 1.376(5) . ?
C9 C10 1.433(5) . ?
C17 C12 1.420(6) . ?
C17 C18 1.418(6) . ?
C17 C16 1.421(5) . ?
C12 C11 1.420(6) . ?
C12 C13 1.410(6) . ?
C18 H18 0.95 . ?
C11 H11 0.95 . ?
C11 C10 1.362(6) . ?
C10 H10 0.95 . ?
C5 C7 1.524(5) . ?
C5 C6 1.536(6) . ?
C5 C8 1.535(5) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C16 H16 0.95 . ?
C16 C15 1.353(7) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C13 H13 0.95 . ?
C13 C14 1.350(7) . ?
C15 H15 0.95 . ?
C15 C14 1.407(8) . ?
C1 C3 1.469(7) . ?
C1 C2 1.468(8) . ?
C1 C4 1.515(10) . ?
C14 H14 0.95 . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C23 C24 1.5287(10) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C24 H24A 0.99 . ?
C24 H24B 0.99 . ?
C24 C25 1.5382(10) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C25 C26 1.5282(10) . ?
C26 H26A 0.99 . ?
C26 H26B 0.99 . ?
O3 C22 1.378(8) . ?
O3 C19 1.356(8) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
C22 C21 1.466(9) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C21 C20 1.5387(10) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C20 C19 1.463(9) . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
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 C7 48.4(4) 7_566 . . . ?
Zn1 O2 C5 C7 -171.0(2) . . . . ?
Zn1 O2 C5 C6 68.5(3) . . . . ?
Zn1 O2 C5 C6 -72.1(3) 7_566 . . . ?
Zn1 O2 C5 C8 167.5(2) 7_566 . . . ?
Zn1 O2 C5 C8 -51.9(4) . . . . ?
Zn1 O1 C1 C3 -67.9(6) . . . . ?
Zn1 O1 C1 C2 165.0(5) . . . . ?
Zn1 O1 C1 C4 53.9(6) . . . . ?
Zn1 C9 C18 K1 64.1(2) . . . 7_566 ?
Zn1 C9 C18 C17 -177.7(3) . . . . ?
Zn1 C9 C10 C11 177.7(4) . . . . ?
K1 O2 C5 C7 -62.4(3) . . . . ?
K1 O2 C5 C6 177.1(2) . . . . ?
K1 O2 C5 C8 56.7(3) . . . . ?
K1 O1 C1 C3 131.2(5) . . . . ?
K1 O1 C1 C2 4.1(7) . . . . ?
K1 O1 C1 C4 -107.0(6) . . . . ?
K1 O4 C23 C24 159.4(5) . . . . ?
K1 O4 C26 C25 -169.5(5) . . . . ?
K1 C9 C18 C17 118.2(4) 7_566 . . . ?
K1 C9 C10 C11 -86.9(5) 7_566 . . . ?
K1 O3 C22 C21 173.7(7) . . . . ?
K1 O3 C19 C20 -161.0(7) . . . . ?
O4 C23 C24 C25 15.9(10) . . . . ?
C17 C12 C11 C10 -2.0(7) . . . . ?
C17 C12 C13 C14 2.0(8) . . . . ?
C17 C16 C15 C14 -1.3(8) . . . . ?
C12 C17 C18 K1 97.0(4) . . . 7_566 ?
C12 C17 C18 C9 -0.3(6) . . . . ?
C12 C17 C16 C15 0.5(7) . . . . ?
C12 C11 C10 C9 0.5(7) . . . . ?
C12 C13 C14 C15 -2.7(9) . . . . ?
C18 C9 C10 C11 1.0(6) . . . . ?
C18 C17 C12 C11 1.9(6) . . . . ?
C18 C17 C12 C13 179.0(4) . . . . ?
C18 C17 C16 C15 -179.3(4) . . . . ?
C11 C12 C13 C14 178.9(5) . . . . ?
C10 C9 C18 K1 -119.3(3) . . . 7_566 ?
C10 C9 C18 C17 -1.1(6) . . . . ?
C16 C17 C12 C11 -177.9(4) . . . . ?
C16 C17 C12 C13 -0.8(6) . . . . ?
C16 C17 C18 K1 -83.2(4) . . . 7_566 ?
C16 C17 C18 C9 179.4(4) . . . . ?
C16 C15 C14 C13 2.4(9) . . . . ?
C13 C12 C11 C10 -178.9(5) . . . . ?
C23 O4 C26 C25 2.0(9) . . . . ?
C23 C24 C25 C26 -14.1(10) . . . . ?
C24 C25 C26 O4 8.2(10) . . . . ?
C26 O4 C23 C24 -11.6(9) . . . . ?
O3 C22 C21 C20 -12.2(13) . . . . ?
C22 O3 C19 C20 10.6(14) . . . . ?
C22 C21 C20 C19 17.2(14) . . . . ?
C21 C20 C19 O3 -17.6(15) . . . . ?
C19 O3 C22 C21 1.7(13) . . . . ?
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
-1.0001 1.0006 -0.9997 0.1358 -0.022 0.0985
-1.0002 1.0003 0.0001 0.1269 -0.0071 0.0204
1.0002 -1.0003 -0.0001 -0.1269 0.0071 -0.0204
-1.0003 1 0.9999 0.1179 0.0077 -0.0577
1.0003 -1 -0.9999 -0.1179 -0.0077 0.0577
0.0001 -1.0007 0.9993 -0.0764 -0.0456 -0.0818
0.0003 -1.0001 -1.0003 -0.0585 -0.0752 0.0744
0.9999 1.0008 -0.9989 0.017 0.1131 0.0651
-0.9999 -1.0008 0.9989 -0.017 -0.1131 -0.0651
-0.9998 -1.0005 -0.0009 -0.0081 -0.1279 0.013
0.9998 1.0005 0.0009 0.0081 0.1279 -0.013
0.9997 1.0002 1.0007 -0.0009 0.1428 -0.0911
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.082 1.000 172.1 39.2 ?
2 0.250 0.418 0.500 172.1 39.2 ?
3 0.750 0.582 0.500 172.1 39.2 ?
4 0.750 0.918 0.000 172.1 39.2 ?
