#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:00:42 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295180 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/23/1572340.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_1572340
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         'C46 H76 K2 N2 O10 Zn2'
_chemical_formula_sum            'C46 H76 K2 N2 O10 Zn2'
_chemical_formula_weight         1026.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-07-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-26 deposited with the CCDC.	2024-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3733(3)
_cell_length_b                   15.7455(3)
_cell_length_c                   18.5165(3)
_cell_measurement_reflns_used    14363
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      78.8650
_cell_measurement_theta_min      4.4050
_cell_volume                     5356.76(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00 -20.00   0.50    0.40    --  -23.00 139.00 175.00  114
  2  ω    -74.00 -16.00   0.50    0.40    --  -23.00 131.00   1.00  116
  3  ω    -95.00   0.00   0.50    0.40    --  -23.00 -77.00 -90.00  190
  4  ω    -70.00 -12.00   0.50    0.40    --  -23.00 125.00-180.00  116
  5  ω    -30.00  53.00   0.50    0.40    --  -23.00  19.00 120.00  166
  6  ω    -27.00  23.00   0.50    0.40    --   47.42 -19.00 -60.00  100
  7  ω    -25.00  40.00   0.50    0.40    --   47.42 -38.00-120.00  130
  8  ω    -27.00  23.00   0.50    0.40    --   47.42 -19.00-150.00  100
  9  ω    101.00 177.00   0.50    4.00    --  113.25  45.00  30.00  152
 10  ω     42.00  68.00   0.50    4.00    --  113.25 -61.00   0.00   52
 11  ω     91.00 177.00   0.50    4.00    --  113.25  77.00 -90.00  172
 12  ω     96.00 177.00   0.50    4.00    --  113.25  64.00 141.86  162
 13  ω     42.00  68.00   0.50    4.00    --  113.25 -61.00  90.00   52
 14  ω     42.00  68.00   0.50    4.00    --  113.25 -61.00  60.00   52
 15  ω     42.00 106.00   0.50    4.00    --  113.25 -98.00-148.67  128
 16  ω     42.00 106.00   0.50    4.00    --  113.25 -94.00-180.00  128
 17  ω     42.00 106.00   0.50    4.00    --  113.25 -94.00-120.00  128
 18  ω     97.00 177.00   0.50    4.00    --  113.25  61.00-120.00  160
 19  ω     42.00  68.00   0.50    4.00    --  113.25 -61.00 -90.00   52
 20  ω     42.00 108.00   0.50    4.00    --  113.25-106.00 -56.58  132
 21  ω     42.00 106.00   0.50    4.00    --  113.25 -94.00 -60.00  128
 22  ω     42.00  68.00   0.50    4.00    --  113.25 -61.00-150.00   52
 23  ω     42.00  68.00   0.50    4.00    --  113.25 -61.00 -60.00   52
 24  ω     42.00 102.00   0.50    4.00    --  113.25 -77.00 150.00  120
 25  ω     42.00 102.00   0.50    4.00    --  113.25 -77.00-120.00  120
 26  ω    101.00 177.00   0.50    4.00    --  113.25  45.00 -60.00  152
 27  ω     91.00 177.00   0.50    4.00    --  113.25  75.00  -8.87  172
 28  ω     25.00  79.00   0.50    0.40    --   47.42  77.00 150.00  108
 29  ω     25.00 119.00   0.50    0.40    --   47.42  77.00   0.00  188
;
_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      -0.0022407000
_diffrn_orient_matrix_UB_12      -0.0552043000
_diffrn_orient_matrix_UB_13      0.0686137000
_diffrn_orient_matrix_UB_21      -0.0078288000
_diffrn_orient_matrix_UB_22      -0.0803302000
_diffrn_orient_matrix_UB_23      -0.0469853000
_diffrn_orient_matrix_UB_31      0.0834104000
_diffrn_orient_matrix_UB_32      -0.0090877000
_diffrn_orient_matrix_UB_33      -0.0024935000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_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            50695
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         4.402
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.909
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.197
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5474
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0685P)²+4.0507P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4842
_reflns_number_total             5474
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc03892d2.cif
_cod_data_source_block           22eh088_nj-3-181
_cod_depositor_comments
'Adding full bibliography for 1572338--1572342.cif.'
_cod_original_cell_volume        5356.74(16)
_cod_database_code               1572340
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H34KNO5Zn
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C18)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
3. Others
 Sof(C19A)=Sof(H19B)=Sof(H19A)=1-FVAR(1)
 Sof(C19)=Sof(H19C)=Sof(H19D)=FVAR(1)
 Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18A)=Sof(H18B)=1-FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18C)=Sof(H18D)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B), C17(H17C,H17D), C17(H17A,H17B), C19A(H19B,
 H19A), C23(H23A,H23B), C20(H20A,H20B), C21(H21A,H21B), C18A(H18A,H18B),
 C19(H19C,H19D), C18(H18C,H18D)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C5(H5), C3(H3)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C)
;
_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 1.802
_oxdiff_exptl_absorpt_empirical_full_min 0.589
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'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 0.03090(2) 0.92887(2) 0.45359(2) 0.04375(13) Uani 1 1 d . . . . .
K1 K -0.13562(3) 0.99664(4) 0.39213(3) 0.05444(17) Uani 1 1 d . . . . .
O3 O 0.17137(11) 0.90627(15) 0.37821(11) 0.0592(5) Uani 1 1 d . . . . .
O4 O -0.17173(14) 1.08438(17) 0.27294(14) 0.0759(7) Uani 1 1 d . . . . .
C11 C 0.04301(17) 1.0758(2) 0.32220(15) 0.0560(7) Uani 1 1 d . . . . .
H11A H -0.005139 1.061040 0.303217 0.084 Uiso 1 1 calc R U . . .
H11B H 0.073502 1.024799 0.323973 0.084 Uiso 1 1 calc R U . . .
H11C H 0.065793 1.118144 0.290648 0.084 Uiso 1 1 calc R U . . .
C12 C -0.03587(17) 0.8017(2) 0.35608(15) 0.0554(7) Uani 1 1 d . . . . .
C8 C 0.03503(15) 1.11249(18) 0.39827(14) 0.0477(6) Uani 1 1 d . . . . .
C10 C -0.01291(18) 1.19188(19) 0.39589(16) 0.0558(7) Uani 1 1 d . . . . .
H10A H 0.010136 1.234952 0.365286 0.084 Uiso 1 1 calc R U . . .
H10B H -0.018893 1.214385 0.444873 0.084 Uiso 1 1 calc R U . . .
H10C H -0.060696 1.177154 0.375975 0.084 Uiso 1 1 calc R U . . .
C14 C 0.0134(2) 0.8233(2) 0.29219(16) 0.0659(8) Uani 1 1 d . . . . .
H14A H 0.018226 0.773499 0.260846 0.099 Uiso 1 1 calc R U . . .
H14B H 0.061532 0.840049 0.310047 0.099 Uiso 1 1 calc R U . . .
H14C H -0.007938 0.870336 0.264717 0.099 Uiso 1 1 calc R U . . .
O5 O -0.26992(17) 0.9207(3) 0.3816(2) 0.1168(13) Uani 1 1 d . . . . .
C4 C 0.38133(19) 0.8809(3) 0.4435(2) 0.0710(9) Uani 1 1 d . . . . .
H4 H 0.429589 0.874134 0.460982 0.085 Uiso 1 1 calc R U . . .
C6 C 0.3007(2) 0.8974(3) 0.3416(2) 0.0763(10) Uani 1 1 d . . . . .
H6 H 0.292693 0.902608 0.291103 0.092 Uiso 1 1 calc R U . . .
C5 C 0.36990(19) 0.8890(3) 0.3706(2) 0.0772(10) Uani 1 1 d . . . . .
H5 H 0.410639 0.888774 0.338960 0.093 Uiso 1 1 calc R U . . .
C3 C 0.32415(18) 0.8823(3) 0.49213(19) 0.0690(9) Uani 1 1 d . . . . .
H3 H 0.332294 0.877679 0.542636 0.083 Uiso 1 1 calc R U . . .
C15 C -0.1111(2) 0.7765(3) 0.3297(2) 0.0779(10) Uani 1 1 d . . . . .
H15A H -0.131712 0.822787 0.300766 0.117 Uiso 1 1 calc R U . . .
H15B H -0.142730 0.765347 0.371226 0.117 Uiso 1 1 calc R U . . .
H15C H -0.107459 0.725173 0.299967 0.117 Uiso 1 1 calc R U . . .
C13 C -0.0041(2) 0.7274(2) 0.39888(18) 0.0675(8) Uani 1 1 d . . . . .
H13A H -0.002251 0.676786 0.368082 0.101 Uiso 1 1 calc R U . . .
H13B H -0.034827 0.715895 0.441012 0.101 Uiso 1 1 calc R U . . .
H13C H 0.045210 0.741771 0.414967 0.101 Uiso 1 1 calc R U . . .
O1 O -0.00003(10) 1.05136(11) 0.44281(9) 0.0441(4) Uani 1 1 d . . . . .
O2 O -0.04413(11) 0.87320(13) 0.40077(10) 0.0522(4) Uani 1 1 d . . . . .
C9 C 0.11006(16) 1.1347(2) 0.42907(16) 0.0548(6) Uani 1 1 d . . . . .
H9A H 0.141077 1.084037 0.428438 0.082 Uiso 1 1 calc R U . . .
H9B H 0.104686 1.154825 0.478861 0.082 Uiso 1 1 calc R U . . .
H9C H 0.132408 1.179322 0.399620 0.082 Uiso 1 1 calc R U . . .
C16 C -0.1368(2) 1.1108(3) 0.2074(2) 0.0820(11) Uani 1 1 d . . . . .
H16A H -0.119715 1.060916 0.179627 0.098 Uiso 1 1 calc R U . . .
H16B H -0.094498 1.147645 0.218143 0.098 Uiso 1 1 calc R U . . .
N1 N 0.18606(14) 0.89662(18) 0.49773(13) 0.0585(6) Uani 1 1 d . . . . .
C1 C 0.13819(16) 0.90602(19) 0.44738(14) 0.0507(6) Uani 1 1 d . . . . .
C2 C 0.25435(17) 0.8909(2) 0.46417(16) 0.0550(7) Uani 1 1 d . . . . .
C7 C 0.24410(17) 0.8977(2) 0.39056(16) 0.0558(7) Uani 1 1 d . . . . .
C22 C -0.3619(4) 0.8794(5) 0.4588(3) 0.129(2) Uani 1 1 d . U . . .
H22A H -0.369634 0.919538 0.499266 0.155 Uiso 1 1 calc R U . . .
H22B H -0.383294 0.823799 0.471903 0.155 Uiso 1 1 calc R U . . .
C17 C -0.1930(2) 1.1589(4) 0.1654(2) 0.1091(18) Uani 1 1 d . . . . .
H17C H -0.200078 1.135487 0.116244 0.131 Uiso 0.245(16) 1 calc R U P A 2
H17D H -0.181897 1.220299 0.162450 0.131 Uiso 0.245(16) 1 calc R U P A 2
H17A H -0.170482 1.201761 0.133308 0.131 Uiso 0.755(16) 1 calc R U P A 1
H17B H -0.223866 1.120305 0.136287 0.131 Uiso 0.755(16) 1 calc R U P A 1
C19A C -0.2411(12) 1.1237(17) 0.2736(13) 0.080(6) Uani 0.44(6) 1 d . U P A 2
H19B H -0.276626 1.085259 0.297089 0.096 Uiso 0.44(6) 1 calc R U P A 2
H19A H -0.238601 1.176517 0.302546 0.096 Uiso 0.44(6) 1 calc R U P A 2
C23 C -0.2850(4) 0.8708(6) 0.4429(4) 0.153(3) Uani 1 1 d . U . . .
H23A H -0.255583 0.890350 0.484490 0.183 Uiso 1 1 calc R U . . .
H23B H -0.272949 0.810556 0.433224 0.183 Uiso 1 1 calc R U . . .
C20 C -0.3345(3) 0.9287(5) 0.3420(3) 0.1191(19) Uani 1 1 d . U . . .
H20A H -0.335260 0.887299 0.301757 0.143 Uiso 1 1 calc R U . . .
H20B H -0.338581 0.986637 0.321556 0.143 Uiso 1 1 calc R U . . .
C21 C -0.3947(3) 0.9122(5) 0.3921(4) 0.134(2) Uani 1 1 d . U . . .
H21A H -0.428626 0.869856 0.371329 0.161 Uiso 1 1 calc R U . . .
H21B H -0.421998 0.965127 0.401929 0.161 Uiso 1 1 calc R U . . .
C18A C -0.2607(11) 1.1395(18) 0.2174(10) 0.085(7) Uani 0.245(16) 1 d . U P A 2
H18A H -0.293111 1.189690 0.219197 0.102 Uiso 0.245(16) 1 calc R U P A 2
H18B H -0.289032 1.091144 0.197836 0.102 Uiso 0.245(16) 1 calc R U P A 2
C19 C -0.2275(11) 1.1476(13) 0.2921(12) 0.100(4) Uani 0.56(6) 1 d . U P A 1
H19C H -0.211411 1.183248 0.333180 0.120 Uiso 0.56(6) 1 calc R U P A 1
H19D H -0.274112 1.119768 0.304894 0.120 Uiso 0.56(6) 1 calc R U P A 1
C18 C -0.2350(5) 1.1994(6) 0.2245(4) 0.104(3) Uani 0.755(16) 1 d . U P A 1
H18C H -0.286978 1.203305 0.210720 0.125 Uiso 0.755(16) 1 calc R U P A 1
H18D H -0.216609 1.257577 0.233074 0.125 Uiso 0.755(16) 1 calc R U P A 1
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'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
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
-7 7 -4 0.0719
-2 -1 0 0.1311
-5 -9 -1 0.1238
0 1 1 0.0983
-2 -1 -1 0.1294
2 0 1 0.1289
-1 1 2 0.0776
0 -1 -2 0.1018
1 0 2 0.1346
2 1 -1 0.1113
-2 -1 1 0.1231
-1 -1 2 0.1159
2 -1 2 0.1320
0 2 1 0.0946
2 -2 -1 0.1554
-1 -2 2 0.1205
1 0 -1 0.1084
0 -1 -1 0.0983
-2 0 1 0.1057
0 1 -2 0.1126
1 2 -1 0.0870
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 61.095(15) 5_576 5_576 ?
Zn1 Zn1 K1 68.040(16) 5_576 . ?
K1 Zn1 K1 129.134(13) . 5_576 ?
O1 Zn1 Zn1 41.16(5) 5_576 5_576 ?
O1 Zn1 Zn1 41.26(5) . 5_576 ?
O1 Zn1 K1 54.56(5) . . ?
O1 Zn1 K1 90.95(5) 5_576 . ?
O1 Zn1 K1 85.33(5) . 5_576 ?
O1 Zn1 K1 49.81(5) 5_576 5_576 ?
O1 Zn1 O1 82.42(7) . 5_576 ?
O2 Zn1 Zn1 111.03(6) . 5_576 ?
O2 Zn1 K1 47.76(6) . . ?
O2 Zn1 K1 159.16(6) . 5_576 ?
O2 Zn1 O1 100.66(8) . . ?
O2 Zn1 O1 110.77(8) . 5_576 ?
O2 Zn1 C1 126.81(10) . . ?
C1 Zn1 Zn1 122.06(9) . 5_576 ?
C1 Zn1 K1 65.38(8) . 5_576 ?
C1 Zn1 K1 155.74(8) . . ?
C1 Zn1 O1 110.92(9) . 5_576 ?
C1 Zn1 O1 116.21(10) . . ?
Zn1 K1 Zn1 50.866(13) . 5_576 ?
Zn1 K1 C23 115.59(13) . . ?
Zn1 K1 C19 145.8(4) . . ?
O4 K1 Zn1 130.69(6) . . ?
O4 K1 Zn1 127.57(7) . 5_576 ?
O4 K1 O5 86.78(10) . . ?
O4 K1 O1 109.70(7) . . ?
O4 K1 N1 102.00(8) . 5_576 ?
O4 K1 C1 119.39(8) . 5_576 ?
O4 K1 C23 108.48(13) . . ?
O4 K1 C19 23.8(3) . . ?
O5 K1 Zn1 132.09(8) . 5_576 ?
O5 K1 Zn1 133.47(9) . . ?
O5 K1 O1 163.11(8) . . ?
O5 K1 N1 90.88(11) . 5_576 ?
O5 K1 C1 104.44(10) . 5_576 ?
O5 K1 C23 21.93(13) . . ?
O5 K1 C19 79.8(4) . . ?
O1 K1 Zn1 33.55(4) . 5_576 ?
O1 K1 Zn1 36.04(4) . . ?
O1 K1 N1 82.28(7) . 5_576 ?
O1 K1 C1 64.75(6) . 5_576 ?
O1 K1 C23 141.21(12) . . ?
O1 K1 C19 113.8(4) . . ?
O2 K1 Zn1 81.33(4) . 5_576 ?
O2 K1 Zn1 33.20(4) . . ?
O2 K1 O4 126.90(7) . . ?
O2 K1 O5 105.20(11) . . ?
O2 K1 O1 68.30(6) . . ?
O2 K1 N1 128.60(7) . 5_576 ?
O2 K1 C1 107.46(7) . 5_576 ?
O2 K1 C23 93.87(15) . . ?
O2 K1 C19 150.7(3) . . ?
N1 K1 Zn1 53.83(5) 5_576 5_576 ?
N1 K1 Zn1 103.88(5) 5_576 . ?
N1 K1 C1 22.04(7) 5_576 5_576 ?
N1 K1 C23 83.40(17) 5_576 . ?
N1 K1 C19 79.4(4) 5_576 . ?
C1 K1 Zn1 81.98(5) 5_576 . ?
C1 K1 Zn1 33.07(5) 5_576 5_576 ?
C1 K1 C23 90.56(16) 5_576 . ?
C1 K1 C19 98.9(4) 5_576 . ?
C23 K1 Zn1 112.63(13) . 5_576 ?
C19 K1 Zn1 117.2(5) . 5_576 ?
C19 K1 C23 98.6(4) . . ?
C7 O3 C1 105.6(2) . . ?
C16 O4 K1 137.2(2) . . ?
C16 O4 C19 108.6(7) . . ?
C19A O4 K1 116.1(6) . . ?
C19A O4 C16 106.4(6) . . ?
C19 O4 K1 108.7(7) . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
C14 C12 C13 110.2(3) . . ?
C15 C12 C14 110.4(3) . . ?
C15 C12 C13 108.4(3) . . ?
O2 C12 C14 109.9(3) . . ?
O2 C12 C15 107.5(3) . . ?
O2 C12 C13 110.4(2) . . ?
C11 C8 C10 109.7(2) . . ?
C11 C8 C9 110.0(2) . . ?
C10 C8 C9 110.0(2) . . ?
O1 C8 C11 108.8(2) . . ?
O1 C8 C10 108.0(2) . . ?
O1 C8 C9 110.2(2) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C23 O5 K1 111.3(3) . . ?
C20 O5 K1 139.3(3) . . ?
C20 O5 C23 107.8(4) . . ?
C5 C4 H4 119.2 . . ?
C5 C4 C3 121.5(3) . . ?
C3 C4 H4 119.2 . . ?
C5 C6 H6 122.0 . . ?
C7 C6 H6 122.0 . . ?
C7 C6 C5 115.9(3) . . ?
C4 C5 C6 122.0(3) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C4 C3 H3 121.3 . . ?
C4 C3 C2 117.4(3) . . ?
C2 C3 H3 121.3 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Zn1 O1 Zn1 97.58(7) . 5_576 ?
Zn1 O1 K1 89.41(7) . . ?
Zn1 O1 K1 96.64(7) 5_576 . ?
C8 O1 Zn1 125.18(16) . . ?
C8 O1 Zn1 124.92(16) . 5_576 ?
C8 O1 K1 114.66(14) . . ?
Zn1 O2 K1 99.04(8) . . ?
C12 O2 Zn1 126.37(18) . . ?
C12 O2 K1 129.70(17) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C16 H16A 110.5 . . ?
O4 C16 H16B 110.5 . . ?
O4 C16 C17 106.1(3) . . ?
H16A C16 H16B 108.7 . . ?
C17 C16 H16A 110.5 . . ?
C17 C16 H16B 110.5 . . ?
C1 N1 K1 103.39(19) . 5_576 ?
C1 N1 C2 107.3(2) . . ?
C2 N1 K1 131.1(2) . 5_576 ?
Zn1 C1 K1 81.55(9) . 5_576 ?
O3 C1 Zn1 118.25(19) . . ?
O3 C1 K1 143.8(2) . 5_576 ?
N1 C1 Zn1 130.4(2) . . ?
N1 C1 K1 54.56(16) . 5_576 ?
N1 C1 O3 111.1(2) . . ?
C3 C2 N1 131.8(3) . . ?
C7 C2 C3 120.1(3) . . ?
C7 C2 N1 108.1(3) . . ?
O3 C7 C6 129.0(3) . . ?
O3 C7 C2 107.9(3) . . ?
C6 C7 C2 123.1(3) . . ?
H22A C22 H22B 108.8 . . ?
C23 C22 H22A 110.7 . . ?
C23 C22 H22B 110.7 . . ?
C23 C22 C21 105.2(5) . . ?
C21 C22 H22A 110.7 . . ?
C21 C22 H22B 110.7 . . ?
C16 C17 H17C 112.3 . . ?
C16 C17 H17D 112.3 . . ?
C16 C17 H17A 111.6 . . ?
C16 C17 H17B 111.6 . . ?
C16 C17 C18A 97.3(7) . . ?
H17C C17 H17D 109.9 . . ?
H17A C17 H17B 109.4 . . ?
C18A C17 H17C 112.3 . . ?
C18A C17 H17D 112.3 . . ?
C18 C17 C16 101.1(4) . . ?
C18 C17 H17A 111.6 . . ?
C18 C17 H17B 111.6 . . ?
O4 C19A H19B 109.2 . . ?
O4 C19A H19A 109.2 . . ?
H19B C19A H19A 107.9 . . ?
C18A C19A O4 112.0(16) . . ?
C18A C19A H19B 109.2 . . ?
C18A C19A H19A 109.2 . . ?
O5 C23 C22 107.7(6) . . ?
O5 C23 H23A 110.2 . . ?
O5 C23 H23B 110.2 . . ?
C22 C23 H23A 110.2 . . ?
C22 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
O5 C20 H20A 110.3 . . ?
O5 C20 H20B 110.3 . . ?
O5 C20 C21 106.9(5) . . ?
H20A C20 H20B 108.6 . . ?
C21 C20 H20A 110.3 . . ?
C21 C20 H20B 110.3 . . ?
C22 C21 H21A 110.4 . . ?
C22 C21 H21B 110.4 . . ?
C20 C21 C22 106.6(5) . . ?
C20 C21 H21A 110.4 . . ?
C20 C21 H21B 110.4 . . ?
H21A C21 H21B 108.6 . . ?
C17 C18A H18A 109.6 . . ?
C17 C18A H18B 109.6 . . ?
C19A C18A C17 110.4(17) . . ?
C19A C18A H18A 109.6 . . ?
C19A C18A H18B 109.6 . . ?
H18A C18A H18B 108.1 . . ?
O4 C19 H19C 111.1 . . ?
O4 C19 H19D 111.1 . . ?
O4 C19 C18 103.3(11) . . ?
H19C C19 H19D 109.1 . . ?
C18 C19 H19C 111.1 . . ?
C18 C19 H19D 111.1 . . ?
C17 C18 C19 109.6(8) . . ?
C17 C18 H18C 109.8 . . ?
C17 C18 H18D 109.8 . . ?
C19 C18 H18C 109.8 . . ?
C19 C18 H18D 109.8 . . ?
H18C C18 H18D 108.2 . . ?
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 3.0430(7) 5_576 ?
Zn1 K1 3.4343(7) . ?
Zn1 K1 3.6384(7) 5_576 ?
Zn1 O1 2.0244(17) 5_576 ?
Zn1 O1 2.0204(18) . ?
Zn1 O2 1.904(2) . ?
Zn1 C1 2.007(3) . ?
K1 O4 2.687(2) . ?
K1 O5 2.749(3) . ?
K1 O1 2.798(2) . ?
K1 O2 2.575(2) . ?
K1 N1 2.801(3) 5_576 ?
K1 C1 3.344(3) 5_576 ?
K1 C23 3.514(7) . ?
K1 C19 3.454(15) . ?
O3 C1 1.419(3) . ?
O3 C7 1.362(4) . ?
O4 C16 1.435(4) . ?
O4 C19A 1.418(16) . ?
O4 C19 1.473(16) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C8 1.529(4) . ?
C12 C14 1.528(4) . ?
C12 C15 1.519(4) . ?
C12 C13 1.529(5) . ?
C12 O2 1.406(3) . ?
C8 C10 1.530(4) . ?
C8 O1 1.422(3) . ?
C8 C9 1.532(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O5 C23 1.408(7) . ?
O5 C20 1.401(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(5) . ?
C4 C3 1.384(5) . ?
C6 H6 0.9500 . ?
C6 C5 1.387(5) . ?
C6 C7 1.379(4) . ?
C5 H5 0.9500 . ?
C3 H3 0.9500 . ?
C3 C2 1.389(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.498(6) . ?
N1 C1 1.290(4) . ?
N1 C2 1.403(4) . ?
C2 C7 1.380(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.450(9) . ?
C22 C21 1.468(8) . ?
C17 H17C 0.9900 . ?
C17 H17D 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18A 1.60(2) . ?
C17 C18 1.484(8) . ?
C19A H19B 0.9900 . ?
C19A H19A 0.9900 . ?
C19A C18A 1.13(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.467(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C19 C18 1.500(17) . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
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
K1 O4 C16 C17 179.9(3) . . . . ?
K1 O4 C19A C18A -160(2) . . . . ?
K1 O4 C19 C18 172.4(11) . . . . ?
K1 O5 C23 C22 143.1(5) . . . . ?
K1 O5 C20 C21 -141.6(5) . . . . ?
K1 N1 C1 Zn1 -32.5(3) 5_576 . . . ?
K1 N1 C1 O3 142.0(2) 5_576 . . . ?
K1 N1 C2 C3 52.1(5) 5_576 . . . ?
K1 N1 C2 C7 -126.3(2) 5_576 . . . ?
O4 C16 C17 C18A -6.9(11) . . . . ?
O4 C16 C17 C18 33.5(7) . . . . ?
O4 C19A C18A C17 -30(3) . . . . ?
O4 C19 C18 C17 8.2(19) . . . . ?
C11 C8 O1 Zn1 -174.97(17) . . . 5_576 ?
C11 C8 O1 Zn1 51.5(3) . . . . ?
C11 C8 O1 K1 -56.6(2) . . . . ?
C10 C8 O1 Zn1 -56.0(3) . . . 5_576 ?
C10 C8 O1 Zn1 170.50(17) . . . . ?
C10 C8 O1 K1 62.5(2) . . . . ?
C14 C12 O2 Zn1 -63.6(3) . . . . ?
C14 C12 O2 K1 86.2(3) . . . . ?
O5 C20 C21 C22 -9.9(8) . . . . ?
C4 C3 C2 N1 -178.2(4) . . . . ?
C4 C3 C2 C7 -0.1(5) . . . . ?
C5 C4 C3 C2 1.0(6) . . . . ?
C5 C6 C7 O3 178.8(4) . . . . ?
C5 C6 C7 C2 0.6(6) . . . . ?
C3 C4 C5 C6 -1.2(7) . . . . ?
C3 C2 C7 O3 -179.3(3) . . . . ?
C3 C2 C7 C6 -0.8(5) . . . . ?
C15 C12 O2 Zn1 176.2(2) . . . . ?
C15 C12 O2 K1 -33.9(4) . . . . ?
C13 C12 O2 Zn1 58.2(3) . . . . ?
C13 C12 O2 K1 -151.9(2) . . . . ?
C9 C8 O1 Zn1 -69.3(3) . . . . ?
C9 C8 O1 Zn1 64.3(3) . . . 5_576 ?
C9 C8 O1 K1 -177.30(17) . . . . ?
C16 O4 C19A C18A 25(3) . . . . ?
C16 O4 C19 C18 13.7(18) . . . . ?
C16 C17 C18A C19A 23(3) . . . . ?
C16 C17 C18 C19 -25.4(14) . . . . ?
N1 C2 C7 O3 -0.7(4) . . . . ?
N1 C2 C7 C6 177.8(3) . . . . ?
C1 O3 C7 C6 -177.4(4) . . . . ?
C1 O3 C7 C2 1.0(3) . . . . ?
C1 N1 C2 C3 178.4(4) . . . . ?
C1 N1 C2 C7 0.1(4) . . . . ?
C2 N1 C1 Zn1 -173.8(2) . . . . ?
C2 N1 C1 K1 -141.4(3) . . . 5_576 ?
C2 N1 C1 O3 0.6(4) . . . . ?
C7 O3 C1 Zn1 174.1(2) . . . . ?
C7 O3 C1 K1 57.3(4) . . . 5_576 ?
C7 O3 C1 N1 -1.0(4) . . . . ?
C7 C6 C5 C4 0.4(7) . . . . ?
C19A O4 C16 C17 -6.9(16) . . . . ?
C23 O5 C20 C21 21.7(8) . . . . ?
C23 C22 C21 C20 -5.1(9) . . . . ?
C20 O5 C23 C22 -25.4(9) . . . . ?
C21 C22 C23 O5 18.4(9) . . . . ?
C19 O4 C16 C17 -30.5(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
-7.0001 7.0000 -4.0000 -0.6452 -0.3196 -0.6375
-2.0000 -1.0000 -0.0000 0.0597 0.0960 -0.1577
-4.9999 -9.0000 -1.0001 0.4394 0.8091 -0.3328
-0.0000 1.0000 1.0000 0.0134 -0.1273 -0.0116
-2.0000 -1.0000 -1.0000 -0.0089 0.1430 -0.1552
2.0000 0.0000 1.0000 0.0641 -0.0626 0.1643
-1.0000 1.0000 2.0000 0.0843 -0.1665 -0.0975
0.0000 -1.0000 -2.0000 -0.0820 0.1743 0.0141
1.0000 0.0000 2.0000 0.1350 -0.1018 0.0784
2.0000 1.0000 -1.0000 -0.1283 -0.0490 0.1602
-2.0000 -1.0000 1.0000 0.1283 0.0490 -0.1602
-1.0000 -1.0000 2.0000 0.1947 -0.0058 -0.0793
2.0000 -1.0000 2.0000 0.1880 -0.0293 0.1709
-0.0000 2.0000 1.0000 -0.0418 -0.2076 -0.0207
2.0001 -2.0000 -1.0000 0.0373 0.1920 0.1875
-1.0000 -2.0000 2.0000 0.2499 0.0745 -0.0702
1.0000 -0.0000 -1.0000 -0.0709 0.0392 0.0859
0.0000 -1.0000 -1.0000 -0.0134 0.1273 0.0116
-2.0000 -0.0000 1.0000 0.0731 -0.0313 -0.1693
-0.0000 1.0000 -2.0000 -0.1924 0.0136 -0.0041
1.0000 2.0000 -1.0000 -0.1813 -0.1215 0.0677
