#------------------------------------------------------------------------------
#$Date: 2022-02-10 00:57:06 +0200 (Thu, 10 Feb 2022) $
#$Revision: 272888 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/96/7129699.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_7129699
loop_
_publ_author_name
'Ozawa, Narito'
'Shivakumar, Kilingaru I.'
'Murugavel, Muthuchamy'
'Inaba, Yuya'
'Yoneda, Tomoki'
'Ide, Yuki'
'Pirillo, Jenny'
'Hijikata, Yuh'
'Inokuma, Yasuhide'
_publ_section_title
;
 Alkali metal ion binding using cyclic polyketones
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00361A
_journal_year                    2022
_chemical_formula_moiety
'C37 H53 K N O10, C24 H16 B Cl4, 0.176(C H Cl3), 1.824(C2 H3 N)'
_chemical_formula_sum            'C64.82 H74.65 B Cl4.53 K N2.82 O10'
_chemical_formula_weight         1263.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-11 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                107.967(2)
_cell_angle_beta                 106.917(2)
_cell_angle_gamma                102.643(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3354(3)
_cell_length_b                   15.5230(4)
_cell_length_c                   16.9525(4)
_cell_measurement_reflns_used    14992
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.9730
_cell_measurement_theta_min      2.1870
_cell_volume                     3229.71(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (sheldrick, 2018)''
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43700
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1329
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         13182
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0564
_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)+(0.0698P)²+3.2239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10282
_reflns_number_total             13182
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc00361a2.cif
_cod_data_source_block           compound_5_KBAr4
_cod_original_cell_volume        3229.71(14)
_cod_database_code               7129699
_shelx_shelxl_version_number     2018/3
_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.
;
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
C1 C 0.9593(2) 0.38640(18) 0.33807(17) 0.0263(5) Uani 1 1 d . . . . .
C2 C 1.0091(2) 0.4663(2) 0.31265(19) 0.0320(6) Uani 1 1 d . . . . .
C3 C 0.9297(2) 0.4571(2) 0.2246(2) 0.0339(6) Uani 1 1 d . . . . .
C4 C 0.9058(2) 0.3721(2) 0.14007(19) 0.0333(6) Uani 1 1 d . . . . .
H1 H 0.879321 0.312022 0.147732 0.040 Uiso 1 1 calc R U . . .
H2 H 0.970351 0.372926 0.129624 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8257(2) 0.3729(2) 0.05843(19) 0.0326(6) Uani 1 1 d . . . . .
H3 H 0.851324 0.434080 0.052208 0.039 Uiso 1 1 calc R U . . .
H4 H 0.817735 0.319598 0.003748 0.039 Uiso 1 1 calc R U . . .
O1 O 0.86604(14) 0.35999(14) 0.31762(13) 0.0324(4) Uani 1 1 d . . . . .
O2 O 0.8885(2) 0.51665(17) 0.22346(16) 0.0545(7) Uani 1 1 d . . . . .
C6 C 0.7212(2) 0.36226(19) 0.06475(17) 0.0261(5) Uani 1 1 d . . . . .
O3 O 0.68985(15) 0.31007(14) 0.09884(13) 0.0319(4) Uani 1 1 d . . . . .
C7 C 0.6518(2) 0.41044(19) 0.02155(17) 0.0254(5) Uani 1 1 d . . . . .
C8 C 0.5663(2) 0.40985(18) 0.05942(17) 0.0254(5) Uani 1 1 d . . . . .
O4 O 0.47615(14) 0.36196(15) 0.01104(13) 0.0332(4) Uani 1 1 d . . . . .
C9 C 0.5965(2) 0.47355(19) 0.15646(18) 0.0277(6) Uani 1 1 d . . . . .
H5 H 0.623196 0.541595 0.164940 0.033 Uiso 1 1 calc R U . . .
H6 H 0.653338 0.459705 0.194339 0.033 Uiso 1 1 calc R U . . .
C10 C 0.5074(2) 0.46040(19) 0.18824(19) 0.0285(6) Uani 1 1 d . . . . .
H7 H 0.530788 0.508658 0.250351 0.034 Uiso 1 1 calc R U . . .
H8 H 0.449716 0.472549 0.149408 0.034 Uiso 1 1 calc R U . . .
C11 C 0.4679(2) 0.36095(18) 0.18648(16) 0.0242(5) Uani 1 1 d . . . . .
O5 O 0.52315(14) 0.31186(14) 0.18894(13) 0.0297(4) Uani 1 1 d . . . . .
C12 C 0.3581(2) 0.32354(19) 0.18221(18) 0.0263(5) Uani 1 1 d . . . . .
C13 C 0.3441(2) 0.22710(19) 0.19334(18) 0.0257(5) Uani 1 1 d . . . . .
O6 O 0.29256(16) 0.15170(14) 0.13022(14) 0.0374(5) Uani 1 1 d . . . . .
C14 C 0.3961(2) 0.2308(2) 0.28631(18) 0.0289(6) Uani 1 1 d . . . . .
H9 H 0.366589 0.265277 0.326874 0.035 Uiso 1 1 calc R U . . .
H10 H 0.471006 0.267590 0.309796 0.035 Uiso 1 1 calc R U . . .
C15 C 0.3826(3) 0.1308(2) 0.2870(2) 0.0346(6) Uani 1 1 d . . . . .
H11 H 0.406677 0.137282 0.350218 0.041 Uiso 1 1 calc R U . . .
H12 H 0.307829 0.092157 0.257689 0.041 Uiso 1 1 calc R U . . .
C16 C 0.4393(2) 0.07775(19) 0.24099(17) 0.0263(5) Uani 1 1 d . . . . .
O7 O 0.50127(15) 0.11634(15) 0.21620(15) 0.0355(5) Uani 1 1 d . . . . .
C17 C 0.4197(2) -0.02877(19) 0.22417(18) 0.0274(6) Uani 1 1 d . . . . .
C18 C 0.5272(2) -0.03993(19) 0.25187(18) 0.0260(5) Uani 1 1 d . . . . .
O8 O 0.55556(16) -0.08588(15) 0.19803(13) 0.0349(4) Uani 1 1 d . . . . .
C19 C 0.5945(2) 0.0080(2) 0.35115(18) 0.0298(6) Uani 1 1 d . . . . .
H13 H 0.567007 -0.029622 0.382116 0.036 Uiso 1 1 calc R U . . .
H14 H 0.590280 0.073078 0.375807 0.036 Uiso 1 1 calc R U . . .
C20 C 0.7078(2) 0.0168(2) 0.37143(19) 0.0305(6) Uani 1 1 d . . . . .
H15 H 0.744587 0.037474 0.436953 0.037 Uiso 1 1 calc R U . . .
H16 H 0.711690 -0.047113 0.340910 0.037 Uiso 1 1 calc R U . . .
C21 C 0.7614(2) 0.08762(18) 0.34128(16) 0.0253(5) Uani 1 1 d . . . . .
O9 O 0.72554(15) 0.14799(14) 0.32714(13) 0.0315(4) Uani 1 1 d . . . . .
C22 C 0.8607(2) 0.08143(19) 0.32862(18) 0.0280(6) Uani 1 1 d . . . . .
C23 C 0.9153(2) 0.1748(2) 0.32285(18) 0.0286(6) Uani 1 1 d . . . . .
C24 C 0.9710(2) 0.2652(2) 0.40812(19) 0.0363(7) Uani 1 1 d . . . . .
H17 H 1.020988 0.252277 0.453345 0.044 Uiso 1 1 calc R U . . .
H18 H 0.919958 0.283170 0.432666 0.044 Uiso 1 1 calc R U . . .
O10 O 0.91492(18) 0.17643(15) 0.25201(14) 0.0420(5) Uani 1 1 d . . . . .
C25 C 1.0280(2) 0.3483(2) 0.3923(2) 0.0395(7) Uani 1 1 d . . . . .
H19 H 1.073752 0.401235 0.451213 0.047 Uiso 1 1 calc R U . . .
H20 H 1.072791 0.327112 0.361134 0.047 Uiso 1 1 calc R U . . .
C26 C 1.1098(2) 0.4613(3) 0.3007(2) 0.0471(8) Uani 1 1 d . . . . .
H21 H 1.163684 0.477019 0.359163 0.071 Uiso 1 1 calc R U . . .
H22 H 1.132073 0.507508 0.275785 0.071 Uiso 1 1 calc R U . . .
H23 H 1.098222 0.396156 0.259585 0.071 Uiso 1 1 calc R U . . .
C27 C 1.0301(3) 0.5619(2) 0.3894(2) 0.0459(8) Uani 1 1 d . . . . .
H24 H 0.964679 0.565392 0.394896 0.069 Uiso 1 1 calc R U . . .
H25 H 1.061211 0.615846 0.376252 0.069 Uiso 1 1 calc R U . . .
H26 H 1.077694 0.565225 0.445953 0.069 Uiso 1 1 calc R U . . .
C28 C 0.6048(2) 0.3499(2) -0.07983(18) 0.0316(6) Uani 1 1 d . . . . .
H27 H 0.660472 0.348153 -0.102178 0.047 Uiso 1 1 calc R U . . .
H28 H 0.559462 0.378542 -0.110349 0.047 Uiso 1 1 calc R U . . .
H29 H 0.564381 0.284242 -0.091871 0.047 Uiso 1 1 calc R U . . .
C29 C 0.7110(2) 0.5153(2) 0.0410(2) 0.0316(6) Uani 1 1 d . . . . .
H30 H 0.754779 0.549444 0.105240 0.047 Uiso 1 1 calc R U . . .
H31 H 0.661359 0.547389 0.024333 0.047 Uiso 1 1 calc R U . . .
H32 H 0.754531 0.515602 0.005917 0.047 Uiso 1 1 calc R U . . .
C30 C 0.2804(2) 0.3059(2) 0.0897(2) 0.0410(7) Uani 1 1 d . . . . .
H33 H 0.289509 0.366896 0.082053 0.062 Uiso 1 1 calc R U . . .
H34 H 0.209625 0.279559 0.085501 0.062 Uiso 1 1 calc R U . . .
H35 H 0.292517 0.260128 0.042462 0.062 Uiso 1 1 calc R U . . .
C31 C 0.3420(3) 0.3972(2) 0.2577(2) 0.0383(7) Uani 1 1 d . . . . .
H36 H 0.399725 0.416855 0.315017 0.057 Uiso 1 1 calc R U . . .
H37 H 0.276819 0.367730 0.261993 0.057 Uiso 1 1 calc R U . . .
H38 H 0.339255 0.453705 0.244041 0.057 Uiso 1 1 calc R U . . .
C32 C 0.3614(2) -0.0638(2) 0.2777(2) 0.0363(7) Uani 1 1 d . . . . .
H39 H 0.397102 -0.021103 0.341567 0.054 Uiso 1 1 calc R U . . .
H40 H 0.359635 -0.129477 0.269755 0.054 Uiso 1 1 calc R U . . .
H41 H 0.290460 -0.063124 0.255811 0.054 Uiso 1 1 calc R U . . .
C33 C 0.3573(2) -0.0866(2) 0.1230(2) 0.0372(7) Uani 1 1 d . . . . .
H42 H 0.288471 -0.080223 0.106817 0.056 Uiso 1 1 calc R U . . .
H43 H 0.349971 -0.154614 0.108064 0.056 Uiso 1 1 calc R U . . .
H44 H 0.393570 -0.061976 0.089399 0.056 Uiso 1 1 calc R U . . .
C34 C 0.8294(2) -0.0034(2) 0.2390(2) 0.0349(6) Uani 1 1 d . . . . .
H45 H 0.789483 0.010401 0.189576 0.052 Uiso 1 1 calc R U . . .
H46 H 0.786920 -0.061879 0.239467 0.052 Uiso 1 1 calc R U . . .
H47 H 0.891798 -0.012935 0.230641 0.052 Uiso 1 1 calc R U . . .
C35 C 0.9312(2) 0.0646(2) 0.4059(2) 0.0353(6) Uani 1 1 d . . . . .
H48 H 0.998705 0.070145 0.401327 0.053 Uiso 1 1 calc R U . . .
H49 H 0.899157 0.000118 0.402183 0.053 Uiso 1 1 calc R U . . .
H50 H 0.940823 0.112894 0.463576 0.053 Uiso 1 1 calc R U . . .
N1 N 0.6373(2) 0.0577(2) 0.08115(17) 0.0401(6) Uani 1 1 d . . . . .
C36 C 0.6076(2) -0.0240(2) 0.04964(18) 0.0325(6) Uani 1 1 d . . . . .
C37 C 0.5708(3) -0.1286(2) 0.0098(2) 0.0416(7) Uani 1 1 d . . . . .
H51 H 0.575271 -0.150976 -0.049295 0.062 Uiso 1 1 calc R U . . .
H52 H 0.498623 -0.153269 0.002935 0.062 Uiso 1 1 calc R U . . .
H53 H 0.613776 -0.152060 0.048869 0.062 Uiso 1 1 calc R U . . .
K1 K 0.67002(4) 0.23250(4) 0.21624(4) 0.02603(13) Uani 1 1 d . . . . .
B1 B 0.6809(2) 0.7442(2) 0.45037(19) 0.0244(6) Uani 1 1 d . . . . .
C38 C 0.67888(19) 0.63616(18) 0.44466(16) 0.0241(5) Uani 1 1 d . . . . .
C39 C 0.7295(2) 0.58404(19) 0.39958(16) 0.0252(5) Uani 1 1 d . . . . .
H54 H 0.764854 0.611638 0.369085 0.030 Uiso 1 1 calc R U . . .
C40 C 0.7304(2) 0.4938(2) 0.39724(17) 0.0282(6) Uani 1 1 d . . . . .
H55 H 0.765582 0.460870 0.365670 0.034 Uiso 1 1 calc R U . . .
C41 C 0.6796(2) 0.45295(19) 0.44150(17) 0.0264(5) Uani 1 1 d . . . . .
C42 C 0.6281(2) 0.5007(2) 0.48754(18) 0.0300(6) Uani 1 1 d . . . . .
H56 H 0.593223 0.472627 0.518106 0.036 Uiso 1 1 calc R U . . .
C43 C 0.6285(2) 0.59032(19) 0.48802(17) 0.0285(6) Uani 1 1 d . . . . .
H57 H 0.592806 0.622513 0.519438 0.034 Uiso 1 1 calc R U . . .
Cl1 Cl 0.68072(6) 0.34006(5) 0.43908(5) 0.03603(17) Uani 1 1 d . . . . .
C44 C 0.7629(2) 0.82563(19) 0.55020(17) 0.0256(5) Uani 1 1 d . . . . .
C45 C 0.80082(19) 0.8045(2) 0.62518(17) 0.0260(5) Uani 1 1 d . . . . .
H58 H 0.786242 0.738845 0.616794 0.031 Uiso 1 1 calc R U . . .
C46 C 0.8591(2) 0.8752(2) 0.71187(18) 0.0287(6) Uani 1 1 d . . . . .
H59 H 0.884243 0.858015 0.761136 0.034 Uiso 1 1 calc R U . . .
C47 C 0.8792(2) 0.9705(2) 0.72423(18) 0.0286(6) Uani 1 1 d . . . . .
C48 C 0.8494(2) 0.9960(2) 0.65229(19) 0.0328(6) Uani 1 1 d . . . . .
H60 H 0.867086 1.061840 0.660948 0.039 Uiso 1 1 calc R U . . .
C49 C 0.7933(2) 0.9241(2) 0.56721(19) 0.0315(6) Uani 1 1 d . . . . .
H61 H 0.774385 0.942169 0.517732 0.038 Uiso 1 1 calc R U . . .
Cl2 Cl 0.94105(6) 1.05983(5) 0.83370(5) 0.03896(18) Uani 1 1 d . . . . .
C50 C 0.5645(2) 0.75282(19) 0.43360(17) 0.0254(5) Uani 1 1 d . . . . .
C51 C 0.5467(2) 0.8381(2) 0.47040(17) 0.0278(6) Uani 1 1 d . . . . .
H62 H 0.605002 0.894328 0.509839 0.033 Uiso 1 1 calc R U . . .
C52 C 0.4487(2) 0.8457(2) 0.45273(19) 0.0327(6) Uani 1 1 d . . . . .
H63 H 0.440656 0.905646 0.479496 0.039 Uiso 1 1 calc R U . . .
C53 C 0.3631(2) 0.7649(2) 0.3958(2) 0.0369(7) Uani 1 1 d . . . . .
C54 C 0.3746(2) 0.6786(2) 0.3559(3) 0.0465(8) Uani 1 1 d . . . . .
H64 H 0.315854 0.623209 0.315406 0.056 Uiso 1 1 calc R U . . .
C55 C 0.4744(2) 0.6738(2) 0.3759(2) 0.0376(7) Uani 1 1 d . . . . .
H65 H 0.481676 0.613500 0.348851 0.045 Uiso 1 1 calc R U . . .
Cl3 Cl 0.23915(7) 0.77309(7) 0.37385(9) 0.0634(3) Uani 1 1 d . . . . .
C56 C 0.7183(2) 0.76186(18) 0.37201(17) 0.0248(5) Uani 1 1 d . . . . .
C57 C 0.8233(2) 0.7867(2) 0.38580(19) 0.0309(6) Uani 1 1 d . . . . .
H66 H 0.872708 0.804115 0.444414 0.037 Uiso 1 1 calc R U . . .
C58 C 0.8590(2) 0.7871(2) 0.3180(2) 0.0339(6) Uani 1 1 d . . . . .
H67 H 0.930872 0.803087 0.329653 0.041 Uiso 1 1 calc R U . . .
C59 C 0.7878(2) 0.76397(19) 0.23343(18) 0.0292(6) Uani 1 1 d . . . . .
C60 C 0.6836(2) 0.74277(19) 0.21629(18) 0.0286(6) Uani 1 1 d . . . . .
H68 H 0.635252 0.729050 0.158281 0.034 Uiso 1 1 calc R U . . .
C61 C 0.6505(2) 0.74181(18) 0.28576(17) 0.0257(5) Uani 1 1 d . . . . .
H69 H 0.578593 0.726830 0.273713 0.031 Uiso 1 1 calc R U . . .
Cl4 Cl 0.83108(7) 0.76431(5) 0.14723(5) 0.04082(19) Uani 1 1 d . . . . .
N3 N 0.9783(4) 0.7955(3) -0.0803(5) 0.152(3) Uani 1 1 d D . . . .
C64 C 1.0400(3) 0.8643(3) -0.0621(3) 0.0675(12) Uani 1 1 d D . . . .
C65 C 1.1167(3) 0.9514(3) -0.0405(2) 0.0530(9) Uani 1 1 d D . . . .
H73 H 1.084777 0.991068 -0.066701 0.080 Uiso 1 1 calc R U . . .
H74 H 1.168585 0.937683 -0.064840 0.080 Uiso 1 1 calc R U . . .
H75 H 1.150326 0.985994 0.024942 0.080 Uiso 1 1 calc R U . . .
N4 N 0.1102(8) 0.5359(4) 0.1073(5) 0.117(3) Uani 0.824(3) 1 d D . P A 1
C66 C 0.0814(5) 0.5904(5) 0.1162(4) 0.0686(15) Uani 0.824(3) 1 d D . P A 1
C67 C 0.0257(5) 0.6555(5) 0.1178(5) 0.0785(18) Uani 0.824(3) 1 d D . P A 1
H76 H 0.000675 0.657734 0.058396 0.118 Uiso 0.824(3) 1 calc R U P A 1
H77 H 0.071446 0.719885 0.162684 0.118 Uiso 0.824(3) 1 calc R U P A 1
H78 H -0.033369 0.634041 0.133397 0.118 Uiso 0.824(3) 1 calc R U P A 1
C68 C 0.0891(16) 0.705(2) 0.1533(14) 0.112(9) Uani 0.176(3) 1 d D U P A 2
H79 H 0.128224 0.774882 0.192222 0.134 Uiso 0.176(3) 1 calc R U P A 2
Cl5 Cl -0.0021(8) 0.6838(8) 0.0389(5) 0.110(4) Uani 0.176(3) 1 d D U P A 2
Cl6 Cl 0.0007(6) 0.6465(7) 0.1975(6) 0.093(3) Uani 0.176(3) 1 d D U P A 2
Cl7 Cl 0.1708(12) 0.632(2) 0.1504(8) 0.234(13) Uani 0.176(3) 1 d D 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 C1 C25 122.2(3) . . ?
O1 C1 C2 119.0(2) . . ?
C25 C1 C2 118.7(2) . . ?
C26 C2 C3 109.6(2) . . ?
C26 C2 C1 113.4(2) . . ?
C3 C2 C1 107.4(2) . . ?
C26 C2 C27 110.2(3) . . ?
C3 C2 C27 110.2(2) . . ?
C1 C2 C27 105.9(2) . . ?
O2 C3 C4 121.2(3) . . ?
O2 C3 C2 120.7(3) . . ?
C4 C3 C2 118.1(2) . . ?
C3 C4 C5 111.9(2) . . ?
C6 C5 C4 112.8(2) . . ?
C1 O1 K1 153.01(18) . . ?
O3 C6 C5 119.8(2) . . ?
O3 C6 C7 120.1(2) . . ?
C5 C6 C7 119.9(2) . . ?
C6 O3 K1 163.08(18) . . ?
C6 C7 C28 106.8(2) . . ?
C6 C7 C8 107.8(2) . . ?
C28 C7 C8 110.6(2) . . ?
C6 C7 C29 112.8(2) . . ?
C28 C7 C29 110.0(2) . . ?
C8 C7 C29 108.9(2) . . ?
O4 C8 C9 121.0(2) . . ?
O4 C8 C7 120.7(2) . . ?
C9 C8 C7 118.3(2) . . ?
C8 C9 C10 113.4(2) . . ?
C11 C10 C9 113.0(2) . . ?
O5 C11 C10 120.3(2) . . ?
O5 C11 C12 120.6(2) . . ?
C10 C11 C12 119.1(2) . . ?
C11 O5 K1 170.00(18) . . ?
C11 C12 C30 108.9(2) . . ?
C11 C12 C13 107.6(2) . . ?
C30 C12 C13 109.2(2) . . ?
C11 C12 C31 110.0(2) . . ?
C30 C12 C31 110.4(2) . . ?
C13 C12 C31 110.6(2) . . ?
O6 C13 C14 121.3(2) . . ?
O6 C13 C12 121.0(2) . . ?
C14 C13 C12 117.7(2) . . ?
C13 C14 C15 112.5(2) . . ?
C16 C15 C14 114.3(2) . . ?
O7 C16 C15 121.8(2) . . ?
O7 C16 C17 118.5(2) . . ?
C15 C16 C17 119.7(2) . . ?
C16 O7 K1 162.2(2) . . ?
C16 C17 C33 106.7(2) . . ?
C16 C17 C32 114.0(2) . . ?
C33 C17 C32 110.1(2) . . ?
C16 C17 C18 106.1(2) . . ?
C33 C17 C18 110.5(2) . . ?
C32 C17 C18 109.3(2) . . ?
O8 C18 C19 121.6(2) . . ?
O8 C18 C17 122.1(2) . . ?
C19 C18 C17 116.2(2) . . ?
C18 C19 C20 113.3(2) . . ?
C21 C20 C19 112.5(2) . . ?
O9 C21 C20 120.5(2) . . ?
O9 C21 C22 121.0(2) . . ?
C20 C21 C22 118.5(2) . . ?
C21 O9 K1 147.22(18) . . ?
C21 C22 C34 107.0(2) . . ?
C21 C22 C23 108.6(2) . . ?
C34 C22 C23 109.1(2) . . ?
C21 C22 C35 110.7(2) . . ?
C34 C22 C35 110.0(2) . . ?
C23 C22 C35 111.2(2) . . ?
O10 C23 C24 120.2(3) . . ?
O10 C23 C22 121.1(3) . . ?
C24 C23 C22 118.7(2) . . ?
C23 C24 C25 112.0(3) . . ?
C1 C25 C24 114.4(2) . . ?
C36 N1 K1 151.3(2) . . ?
N1 C36 C37 179.3(4) . . ?
O9 K1 O5 131.05(6) . . ?
O9 K1 O3 155.22(6) . . ?
O5 K1 O3 73.42(6) . . ?
O9 K1 O7 69.99(6) . . ?
O5 K1 O7 72.81(6) . . ?
O3 K1 O7 130.06(7) . . ?
O9 K1 O1 82.45(6) . . ?
O5 K1 O1 114.95(6) . . ?
O3 K1 O1 82.43(6) . . ?
O7 K1 O1 145.80(7) . . ?
O9 K1 N1 84.93(7) . . ?
O5 K1 N1 117.22(7) . . ?
O3 K1 N1 85.77(7) . . ?
O7 K1 N1 78.29(7) . . ?
O1 K1 N1 120.01(7) . . ?
O9 K1 Cl1 62.30(5) . . ?
O5 K1 Cl1 78.76(4) . . ?
O3 K1 Cl1 130.59(5) . . ?
O7 K1 Cl1 75.97(5) . . ?
O1 K1 Cl1 73.40(5) . . ?
N1 K1 Cl1 143.61(6) . . ?
C38 B1 C56 107.7(2) . . ?
C38 B1 C44 109.8(2) . . ?
C56 B1 C44 110.0(2) . . ?
C38 B1 C50 110.5(2) . . ?
C56 B1 C50 109.8(2) . . ?
C44 B1 C50 109.0(2) . . ?
C39 C38 C43 114.7(2) . . ?
C39 C38 B1 123.4(2) . . ?
C43 C38 B1 121.9(2) . . ?
C40 C39 C38 123.3(2) . . ?
C41 C40 C39 119.0(2) . . ?
C40 C41 C42 120.7(2) . . ?
C40 C41 Cl1 119.3(2) . . ?
C42 C41 Cl1 120.0(2) . . ?
C41 C42 C43 118.6(2) . . ?
C42 C43 C38 123.7(2) . . ?
C41 Cl1 K1 99.04(9) . . ?
C45 C44 C49 114.9(2) . . ?
C45 C44 B1 123.9(2) . . ?
C49 C44 B1 121.1(2) . . ?
C46 C45 C44 123.2(3) . . ?
C47 C46 C45 118.4(2) . . ?
C48 C47 C46 121.1(2) . . ?
C48 C47 Cl2 119.8(2) . . ?
C46 C47 Cl2 119.1(2) . . ?
C47 C48 C49 118.8(3) . . ?
C48 C49 C44 123.4(3) . . ?
C51 C50 C55 114.3(3) . . ?
C51 C50 B1 124.1(2) . . ?
C55 C50 B1 121.5(2) . . ?
C52 C51 C50 123.7(3) . . ?
C53 C52 C51 119.0(3) . . ?
C54 C53 C52 120.5(3) . . ?
C54 C53 Cl3 119.9(3) . . ?
C52 C53 Cl3 119.5(2) . . ?
C53 C54 C55 118.7(3) . . ?
C54 C55 C50 123.7(3) . . ?
C61 C56 C57 115.5(2) . . ?
C61 C56 B1 124.0(2) . . ?
C57 C56 B1 120.0(2) . . ?
C58 C57 C56 123.2(3) . . ?
C59 C58 C57 118.5(3) . . ?
C60 C59 C58 121.2(2) . . ?
C60 C59 Cl4 119.6(2) . . ?
C58 C59 Cl4 119.2(2) . . ?
C59 C60 C61 118.7(2) . . ?
C56 C61 C60 122.9(2) . . ?
N3 C64 C65 178.9(7) . . ?
N4 C66 C67 170.7(10) . . ?
Cl7 C68 Cl6 100.2(11) . . ?
Cl7 C68 Cl5 113.4(12) . . ?
Cl6 C68 Cl5 102.3(11) . . ?
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
C1 O1 1.216(3) . ?
C1 C25 1.493(4) . ?
C1 C2 1.535(4) . ?
C2 C26 1.530(4) . ?
C2 C3 1.534(4) . ?
C2 C27 1.539(4) . ?
C3 O2 1.203(4) . ?
C3 C4 1.503(4) . ?
C4 C5 1.524(4) . ?
C5 C6 1.510(4) . ?
O1 K1 2.725(2) . ?
C6 O3 1.214(3) . ?
C6 C7 1.525(4) . ?
O3 K1 2.6739(19) . ?
C7 C28 1.531(4) . ?
C7 C8 1.539(4) . ?
C7 C29 1.542(4) . ?
C8 O4 1.218(3) . ?
C8 C9 1.505(4) . ?
C9 C10 1.523(4) . ?
C10 C11 1.511(4) . ?
C11 O5 1.214(3) . ?
C11 C12 1.526(4) . ?
O5 K1 2.6617(19) . ?
C12 C30 1.537(4) . ?
C12 C13 1.543(4) . ?
C12 C31 1.543(4) . ?
C13 O6 1.204(3) . ?
C13 C14 1.512(4) . ?
C14 C15 1.525(4) . ?
C15 C16 1.489(4) . ?
C16 O7 1.210(3) . ?
C16 C17 1.534(4) . ?
O7 K1 2.682(2) . ?
C17 C33 1.534(4) . ?
C17 C32 1.536(4) . ?
C17 C18 1.541(4) . ?
C18 O8 1.203(3) . ?
C18 C19 1.512(4) . ?
C19 C20 1.525(4) . ?
C20 C21 1.505(4) . ?
C21 O9 1.216(3) . ?
C21 C22 1.519(4) . ?
O9 K1 2.6452(19) . ?
C22 C34 1.534(4) . ?
C22 C23 1.535(4) . ?
C22 C35 1.537(4) . ?
C23 O10 1.207(3) . ?
C23 C24 1.511(4) . ?
C24 C25 1.512(4) . ?
N1 C36 1.135(4) . ?
N1 K1 2.795(3) . ?
C36 C37 1.453(4) . ?
K1 Cl1 3.5696(10) . ?
B1 C38 1.644(4) . ?
B1 C56 1.644(4) . ?
B1 C44 1.648(4) . ?
B1 C50 1.651(4) . ?
C38 C39 1.401(4) . ?
C38 C43 1.405(4) . ?
C39 C40 1.392(4) . ?
C40 C41 1.381(4) . ?
C41 C42 1.386(4) . ?
C41 Cl1 1.744(3) . ?
C42 C43 1.388(4) . ?
C44 C45 1.397(4) . ?
C44 C49 1.404(4) . ?
C45 C46 1.397(4) . ?
C46 C47 1.379(4) . ?
C47 C48 1.377(4) . ?
C47 Cl2 1.752(3) . ?
C48 C49 1.383(4) . ?
C50 C51 1.392(4) . ?
C50 C55 1.400(4) . ?
C51 C52 1.389(4) . ?
C52 C53 1.378(4) . ?
C53 C54 1.372(4) . ?
C53 Cl3 1.748(3) . ?
C54 C55 1.395(4) . ?
C56 C61 1.392(4) . ?
C56 C57 1.398(4) . ?
C57 C58 1.388(4) . ?
C58 C59 1.377(4) . ?
C59 C60 1.377(4) . ?
C59 Cl4 1.747(3) . ?
C60 C61 1.395(4) . ?
N3 C64 1.114(6) . ?
C64 C65 1.407(5) . ?
N4 C66 1.010(8) . ?
C66 C67 1.417(8) . ?
C68 Cl7 1.801(19) . ?
C68 Cl6 1.861(19) . ?
C68 Cl5 1.875(18) . ?
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
O1 C1 C2 C26 -153.0(3) . . . . ?
C25 C1 C2 C26 30.9(4) . . . . ?
O1 C1 C2 C3 -31.7(3) . . . . ?
C25 C1 C2 C3 152.2(3) . . . . ?
O1 C1 C2 C27 86.1(3) . . . . ?
C25 C1 C2 C27 -90.0(3) . . . . ?
C26 C2 C3 O2 -126.0(3) . . . . ?
C1 C2 C3 O2 110.4(3) . . . . ?
C27 C2 C3 O2 -4.6(4) . . . . ?
C26 C2 C3 C4 53.5(3) . . . . ?
C1 C2 C3 C4 -70.1(3) . . . . ?
C27 C2 C3 C4 175.0(3) . . . . ?
O2 C3 C4 C5 -0.5(4) . . . . ?
C2 C3 C4 C5 180.0(2) . . . . ?
C3 C4 C5 C6 -64.3(3) . . . . ?
C25 C1 O1 K1 -78.5(5) . . . . ?
C2 C1 O1 K1 105.5(4) . . . . ?
C4 C5 C6 O3 -36.6(4) . . . . ?
C4 C5 C6 C7 148.4(3) . . . . ?
C5 C6 O3 K1 62.7(7) . . . . ?
C7 C6 O3 K1 -122.3(6) . . . . ?
O3 C6 C7 C28 -99.2(3) . . . . ?
C5 C6 C7 C28 75.8(3) . . . . ?
O3 C6 C7 C8 19.7(3) . . . . ?
C5 C6 C7 C8 -165.4(2) . . . . ?
O3 C6 C7 C29 139.9(3) . . . . ?
C5 C6 C7 C29 -45.1(3) . . . . ?
C6 C7 C8 O4 -113.3(3) . . . . ?
C28 C7 C8 O4 3.1(3) . . . . ?
C29 C7 C8 O4 124.1(3) . . . . ?
C6 C7 C8 C9 69.6(3) . . . . ?
C28 C7 C8 C9 -174.0(2) . . . . ?
C29 C7 C8 C9 -53.1(3) . . . . ?
O4 C8 C9 C10 7.9(3) . . . . ?
C7 C8 C9 C10 -175.0(2) . . . . ?
C8 C9 C10 C11 64.2(3) . . . . ?
C9 C10 C11 O5 22.7(3) . . . . ?
C9 C10 C11 C12 -157.7(2) . . . . ?
C10 C11 O5 K1 42.9(11) . . . . ?
C12 C11 O5 K1 -136.7(9) . . . . ?
O5 C11 C12 C30 -111.6(3) . . . . ?
C10 C11 C12 C30 68.8(3) . . . . ?
O5 C11 C12 C13 6.6(3) . . . . ?
C10 C11 C12 C13 -173.0(2) . . . . ?
O5 C11 C12 C31 127.2(3) . . . . ?
C10 C11 C12 C31 -52.4(3) . . . . ?
C11 C12 C13 O6 -106.0(3) . . . . ?
C30 C12 C13 O6 12.0(3) . . . . ?
C31 C12 C13 O6 133.8(3) . . . . ?
C11 C12 C13 C14 74.9(3) . . . . ?
C30 C12 C13 C14 -167.1(2) . . . . ?
C31 C12 C13 C14 -45.3(3) . . . . ?
O6 C13 C14 C15 4.8(4) . . . . ?
C12 C13 C14 C15 -176.1(2) . . . . ?
C13 C14 C15 C16 68.6(3) . . . . ?
C14 C15 C16 O7 9.3(4) . . . . ?
C14 C15 C16 C17 -170.8(2) . . . . ?
C15 C16 O7 K1 65.9(7) . . . . ?
C17 C16 O7 K1 -114.0(6) . . . . ?
O7 C16 C17 C33 -72.5(3) . . . . ?
C15 C16 C17 C33 107.6(3) . . . . ?
O7 C16 C17 C32 165.8(2) . . . . ?
C15 C16 C17 C32 -14.2(4) . . . . ?
O7 C16 C17 C18 45.4(3) . . . . ?
C15 C16 C17 C18 -134.5(3) . . . . ?
C16 C17 C18 O8 -113.0(3) . . . . ?
C33 C17 C18 O8 2.4(4) . . . . ?
C32 C17 C18 O8 123.7(3) . . . . ?
C16 C17 C18 C19 68.6(3) . . . . ?
C33 C17 C18 C19 -176.0(2) . . . . ?
C32 C17 C18 C19 -54.8(3) . . . . ?
O8 C18 C19 C20 16.6(4) . . . . ?
C17 C18 C19 C20 -165.0(2) . . . . ?
C18 C19 C20 C21 69.0(3) . . . . ?
C19 C20 C21 O9 19.2(4) . . . . ?
C19 C20 C21 C22 -160.5(2) . . . . ?
C20 C21 O9 K1 -130.6(3) . . . . ?
C22 C21 O9 K1 49.1(4) . . . . ?
O9 C21 C22 C34 -102.5(3) . . . . ?
C20 C21 C22 C34 77.3(3) . . . . ?
O9 C21 C22 C23 15.2(3) . . . . ?
C20 C21 C22 C23 -165.1(2) . . . . ?
O9 C21 C22 C35 137.6(3) . . . . ?
C20 C21 C22 C35 -42.7(3) . . . . ?
C21 C22 C23 O10 -105.6(3) . . . . ?
C34 C22 C23 O10 10.7(4) . . . . ?
C35 C22 C23 O10 132.3(3) . . . . ?
C21 C22 C23 C24 75.0(3) . . . . ?
C34 C22 C23 C24 -168.6(2) . . . . ?
C35 C22 C23 C24 -47.1(3) . . . . ?
O10 C23 C24 C25 -4.2(4) . . . . ?
C22 C23 C24 C25 175.1(2) . . . . ?
O1 C1 C25 C24 8.0(4) . . . . ?
C2 C1 C25 C24 -176.0(3) . . . . ?
C23 C24 C25 C1 69.3(4) . . . . ?
C56 B1 C38 C39 17.0(3) . . . . ?
C44 B1 C38 C39 -102.8(3) . . . . ?
C50 B1 C38 C39 136.9(2) . . . . ?
C56 B1 C38 C43 -165.4(2) . . . . ?
C44 B1 C38 C43 74.9(3) . . . . ?
C50 B1 C38 C43 -45.4(3) . . . . ?
C43 C38 C39 C40 0.0(4) . . . . ?
B1 C38 C39 C40 177.9(2) . . . . ?
C38 C39 C40 C41 -0.2(4) . . . . ?
C39 C40 C41 C42 0.1(4) . . . . ?
C39 C40 C41 Cl1 -179.87(19) . . . . ?
C40 C41 C42 C43 0.1(4) . . . . ?
Cl1 C41 C42 C43 -179.9(2) . . . . ?
C41 C42 C43 C38 -0.3(4) . . . . ?
C39 C38 C43 C42 0.2(4) . . . . ?
B1 C38 C43 C42 -177.6(2) . . . . ?
C40 C41 Cl1 K1 -35.6(2) . . . . ?
C42 C41 Cl1 K1 144.4(2) . . . . ?
C38 B1 C44 C45 -16.9(3) . . . . ?
C56 B1 C44 C45 -135.3(2) . . . . ?
C50 B1 C44 C45 104.3(3) . . . . ?
C38 B1 C44 C49 168.3(2) . . . . ?
C56 B1 C44 C49 50.0(3) . . . . ?
C50 B1 C44 C49 -70.5(3) . . . . ?
C49 C44 C45 C46 3.9(4) . . . . ?
B1 C44 C45 C46 -171.2(2) . . . . ?
C44 C45 C46 C47 0.7(4) . . . . ?
C45 C46 C47 C48 -4.7(4) . . . . ?
C45 C46 C47 Cl2 173.8(2) . . . . ?
C46 C47 C48 C49 3.7(4) . . . . ?
Cl2 C47 C48 C49 -174.8(2) . . . . ?
C47 C48 C49 C44 1.4(4) . . . . ?
C45 C44 C49 C48 -5.0(4) . . . . ?
B1 C44 C49 C48 170.2(3) . . . . ?
C38 B1 C50 C51 150.8(2) . . . . ?
C56 B1 C50 C51 -90.5(3) . . . . ?
C44 B1 C50 C51 30.0(3) . . . . ?
C38 B1 C50 C55 -32.8(3) . . . . ?
C56 B1 C50 C55 85.9(3) . . . . ?
C44 B1 C50 C55 -153.6(3) . . . . ?
C55 C50 C51 C52 0.4(4) . . . . ?
B1 C50 C51 C52 177.0(2) . . . . ?
C50 C51 C52 C53 0.1(4) . . . . ?
C51 C52 C53 C54 -1.1(4) . . . . ?
C51 C52 C53 Cl3 179.4(2) . . . . ?
C52 C53 C54 C55 1.6(5) . . . . ?
Cl3 C53 C54 C55 -178.9(3) . . . . ?
C53 C54 C55 C50 -1.2(5) . . . . ?
C51 C50 C55 C54 0.2(4) . . . . ?
B1 C50 C55 C54 -176.5(3) . . . . ?
C38 B1 C56 C61 92.6(3) . . . . ?
C44 B1 C56 C61 -147.7(2) . . . . ?
C50 B1 C56 C61 -27.8(3) . . . . ?
C38 B1 C56 C57 -78.8(3) . . . . ?
C44 B1 C56 C57 40.9(3) . . . . ?
C50 B1 C56 C57 160.8(2) . . . . ?
C61 C56 C57 C58 -3.1(4) . . . . ?
B1 C56 C57 C58 169.0(3) . . . . ?
C56 C57 C58 C59 1.4(4) . . . . ?
C57 C58 C59 C60 1.4(4) . . . . ?
C57 C58 C59 Cl4 179.9(2) . . . . ?
C58 C59 C60 C61 -2.2(4) . . . . ?
Cl4 C59 C60 C61 179.3(2) . . . . ?
C57 C56 C61 C60 2.2(4) . . . . ?
B1 C56 C61 C60 -169.5(2) . . . . ?
C59 C60 C61 C56 0.3(4) . . . . ?
