#------------------------------------------------------------------------------
#$Date: 2017-08-10 04:17:49 +0300 (Thu, 10 Aug 2017) $
#$Revision: 199687 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/05/7120530.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_7120530
loop_
_publ_author_name
'Yu, Lirong'
'Li, Yanglizhi'
'Wang, Xi'
'Wang, Xingyong'
'Zhou, Panpan'
'Jiang, ShangDa'
'pan, xiaobo'
_publ_section_title
;
 Consecutive reduction, radical-cyclization, and oxidative-dehydrogenation
 reaction of ortho-substituted diboryl compound
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05689C
_journal_year                    2017
_chemical_formula_moiety         '2(C20 H40 K O8), C54 H56 B2, 2(C4 H8 O)'
_chemical_formula_sum            'C102 H152 B2 K2 O18'
_chemical_formula_weight         1766.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                104.712(4)
_cell_angle_beta                 107.141(4)
_cell_angle_gamma                103.546(4)
_cell_formula_units_Z            1
_cell_length_a                   12.8138(5)
_cell_length_b                   13.8501(6)
_cell_length_c                   16.3243(7)
_cell_measurement_reflns_used    3489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.424
_cell_measurement_theta_min      3.780
_cell_volume                     2523.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -18.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  -99.0000   60.0000 43

#__ type_ start__ end____ width___ exp.time_
  2 omega -102.00  -77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5055  178.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega  -47.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -38.0000    0.0000 101

#__ type_ start__ end____ width___ exp.time_
  4 omega  -45.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -38.0000   90.0000 98

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
  6 omega   16.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000  -60.0000 61

#__ type_ start__ end____ width___ exp.time_
  7 omega   17.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000   30.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0518472000
_diffrn_orient_matrix_UB_12      0.0105950000
_diffrn_orient_matrix_UB_13      0.0372133000
_diffrn_orient_matrix_UB_21      0.0228659000
_diffrn_orient_matrix_UB_22      0.0502374000
_diffrn_orient_matrix_UB_23      -0.0030460000
_diffrn_orient_matrix_UB_31      -0.0238130000
_diffrn_orient_matrix_UB_32      0.0228138000
_diffrn_orient_matrix_UB_33      0.0309466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18549
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         9906
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1349P)²+2.2114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2362
_refine_ls_wR_factor_ref         0.2779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6178
_reflns_number_total             9906
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc05689c2.cif
_cod_data_source_block           yulr_1213_2
_cod_database_code               7120530
_shelx_shelxl_version_number     2014/7
_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.
;
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(C55) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C47) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: H44C(0.4) H44D(0.4) H44A(0.6) H44B(0.6) H51C(0.5) H51D(0.5)
 H51A(0.5) H51B(0.5) H53A(0.5) H53B(0.5) H53C(0.5) H53D(0.5) O10(0.5) C48(0.6)
 H48A(0.6) H48B(0.6) C49(0.6) H49A(0.6) H49B(0.6) C50(0.6) H50A(0.6) H50B(0.6)
 C54(0.65) H54A(0.65) H54B(0.65) O9(0.5) C45(0.4) H45A(0.4) H45B(0.4) C46(0.4)
 H46A(0.4) H46B(0.4) C47(0.4) H47A(0.4) H47B(0.4) C55(0.35) H55A(0.35)
 H55B(0.35)
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C44(H44C,H44D), C44(H44A,H44B),
  C51(H51C,H51D), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C53(H53C,
 H53D), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C54(H54A,H54B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C55(H55A,H55B), C40(H40A,H40B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C12(H12), C14(H14), C21(H21), C23(H23)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_olex2_date_sample_data_collection 2016-12-13
_olex2_submission_special_instructions 'No special instructions were received'
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
K1 K 0.03185(7) 0.72587(6) 0.28634(5) 0.0369(2) Uani 1 1 d . . . . .
O1 O 0.2364(3) 0.8371(2) 0.2710(2) 0.0603(9) Uani 1 1 d . . . . .
O2 O 0.0177(3) 0.7821(3) 0.1306(2) 0.0631(9) Uani 1 1 d . . . . .
O3 O -0.1847(3) 0.7123(3) 0.1669(2) 0.0658(9) Uani 1 1 d . . . . .
O4 O -0.1699(3) 0.6163(3) 0.3019(2) 0.0595(8) Uani 1 1 d . . . . .
O5 O 0.0463(3) 0.6721(2) 0.4444(2) 0.0556(8) Uani 1 1 d . . . . .
O6 O 0.2435(3) 0.7368(3) 0.4034(2) 0.0619(9) Uani 1 1 d . . . . .
O7 O 0.0358(3) 0.9214(3) 0.3805(3) 0.0704(10) Uani 1 1 d . . . . .
C28 C 0.2236(5) 0.8320(4) 0.1831(4) 0.0736(16) Uani 1 1 d . . . . .
H28A H 0.2157 0.7597 0.1467 0.088 Uiso 1 1 calc R . . . .
H28B H 0.2936 0.8822 0.1842 0.088 Uiso 1 1 calc R . . . .
C29 C 0.1182(5) 0.8588(4) 0.1386(3) 0.0651(14) Uani 1 1 d . . . . .
H29A H 0.1240 0.9298 0.1761 0.078 Uiso 1 1 calc R . . . .
H29B H 0.1137 0.8600 0.0773 0.078 Uiso 1 1 calc R . . . .
C30 C -0.0847(6) 0.8014(5) 0.0895(4) 0.0795(18) Uani 1 1 d . . . . .
H30A H -0.0903 0.8052 0.0287 0.095 Uiso 1 1 calc R . . . .
H30B H -0.0837 0.8700 0.1278 0.095 Uiso 1 1 calc R . . . .
C31 C -0.1873(5) 0.7135(5) 0.0795(3) 0.0732(15) Uani 1 1 d . . . . .
H31A H -0.2597 0.7236 0.0461 0.088 Uiso 1 1 calc R . . . .
H31B H -0.1860 0.6448 0.0435 0.088 Uiso 1 1 calc R . . . .
C32 C -0.2760(4) 0.6295(5) 0.1606(4) 0.0756(16) Uani 1 1 d . . . . .
H32A H -0.2718 0.5608 0.1276 0.091 Uiso 1 1 calc R . . . .
H32B H -0.3509 0.6352 0.1263 0.091 Uiso 1 1 calc R . . . .
C33 C -0.2678(4) 0.6355(5) 0.2563(4) 0.0716(15) Uani 1 1 d . . . . .
H33A H -0.2652 0.7067 0.2906 0.086 Uiso 1 1 calc R . . . .
H33B H -0.3374 0.5827 0.2530 0.086 Uiso 1 1 calc R . . . .
C34 C -0.1592(5) 0.6242(4) 0.3903(4) 0.0690(15) Uani 1 1 d . . . . .
H34A H -0.2290 0.5743 0.3896 0.083 Uiso 1 1 calc R . . . .
H34B H -0.1515 0.6969 0.4255 0.083 Uiso 1 1 calc R . . . .
C35 C -0.0520(5) 0.5979(4) 0.4352(4) 0.0627(13) Uani 1 1 d . . . . .
H35A H -0.0481 0.5957 0.4961 0.075 Uiso 1 1 calc R . . . .
H35B H -0.0576 0.5271 0.3974 0.075 Uiso 1 1 calc R . . . .
C36 C 0.1456(5) 0.6481(5) 0.4809(3) 0.0685(14) Uani 1 1 d . . . . .
H36A H 0.1403 0.5790 0.4402 0.082 Uiso 1 1 calc R . . . .
H36B H 0.1524 0.6424 0.5414 0.082 Uiso 1 1 calc R . . . .
C37 C 0.2498(5) 0.7322(5) 0.4909(3) 0.0702(15) Uani 1 1 d . . . . .
H37A H 0.2543 0.8015 0.5306 0.084 Uiso 1 1 calc R . . . .
H37B H 0.3205 0.7169 0.5200 0.084 Uiso 1 1 calc R . . . .
C38 C 0.3392(4) 0.8092(4) 0.4058(4) 0.0688(14) Uani 1 1 d . . . . .
H38A H 0.4097 0.7943 0.4363 0.083 Uiso 1 1 calc R . . . .
H38B H 0.3462 0.8813 0.4419 0.083 Uiso 1 1 calc R . . . .
C39 C 0.3305(4) 0.8046(4) 0.3119(4) 0.0645(13) Uani 1 1 d . . . . .
H39A H 0.4037 0.8517 0.3147 0.077 Uiso 1 1 calc R . . . .
H39B H 0.3181 0.7314 0.2744 0.077 Uiso 1 1 calc R . . . .
C44 C 0.1473(6) 0.9786(5) 0.4463(5) 0.103(2) Uani 1 1 d . . . . .
H44C H 0.2096 0.9654 0.4256 0.124 Uiso 0.4 1 calc R . P A 2
H44D H 0.1585 0.9697 0.5063 0.124 Uiso 0.4 1 calc R . P A 2
H44A H 0.2036 0.9829 0.4157 0.124 Uiso 0.6 1 calc R . P B 1
H44B H 0.1671 0.9402 0.4891 0.124 Uiso 0.6 1 calc R . P B 1
C51 C 0.1294(7) 0.5000(5) 0.2053(6) 0.111(3) Uani 1 1 d . . . . .
H51C H 0.2058 0.5500 0.2169 0.134 Uiso 0.5 1 calc R . P C 2
H51D H 0.1335 0.4790 0.2594 0.134 Uiso 0.5 1 calc R . P C 2
H51A H 0.1731 0.4843 0.2584 0.134 Uiso 0.5 1 calc R . P D 1
H51B H 0.1829 0.5604 0.2000 0.134 Uiso 0.5 1 calc R . P D 1
C52 C 0.0919(6) 0.4086(5) 0.1234(4) 0.0772(16) Uani 1 1 d . . . . .
H52A H 0.1153 0.3499 0.1382 0.093 Uiso 1 1 calc R . . . .
H52B H 0.1246 0.4267 0.0792 0.093 Uiso 1 1 calc R . . . .
C53 C -0.0361(8) 0.3799(7) 0.0866(6) 0.149(4) Uani 1 1 d . . . . .
H53A H -0.0747 0.3028 0.0690 0.179 Uiso 0.5 1 calc R . P E 1
H53B H -0.0633 0.4018 0.0332 0.179 Uiso 0.5 1 calc R . P E 1
H53C H -0.0727 0.3421 0.1203 0.179 Uiso 0.5 1 calc R . P F 2
H53D H -0.0717 0.3381 0.0204 0.179 Uiso 0.5 1 calc R . P F 2
O10 O 0.0422(9) 0.5290(9) 0.2213(7) 0.085(3) Uani 0.5 1 d . U P G 1
C48 C 0.1580(9) 1.0858(7) 0.4983(7) 0.062(2) Uani 0.6 1 d . U P H 1
H48A H 0.2370 1.1365 0.5182 0.075 Uiso 0.6 1 calc R . P H 1
H48B H 0.1362 1.0880 0.5519 0.075 Uiso 0.6 1 calc R . P H 1
C49 C 0.0697(13) 1.1051(9) 0.4244(8) 0.064(3) Uani 0.6 1 d . U P H 1
H49A H 0.0094 1.1231 0.4454 0.077 Uiso 0.6 1 calc R . P H 1
H49B H 0.1077 1.1636 0.4073 0.077 Uiso 0.6 1 calc R . P H 1
C50 C 0.0180(11) 1.0021(8) 0.3449(6) 0.069(2) Uani 0.6 1 d . U P H 1
H50A H -0.0658 0.9874 0.3132 0.082 Uiso 0.6 1 calc R . P H 1
H50B H 0.0562 1.0055 0.3006 0.082 Uiso 0.6 1 calc R . P H 1
C54 C -0.0576(11) 0.4425(10) 0.1676(10) 0.121(4) Uani 0.65 1 d . U P G 1
H54A H -0.1242 0.4667 0.1458 0.146 Uiso 0.65 1 calc R . P G 1
H54B H -0.0755 0.3976 0.2034 0.146 Uiso 0.65 1 calc R . P G 1
O9 O 0.0365(12) 0.5463(8) 0.1817(7) 0.083(3) Uani 0.5 1 d . U P G 2
C45 C 0.126(2) 1.1029(16) 0.4429(18) 0.088(6) Uani 0.4 1 d . U P H 2
H45A H 0.1594 1.1561 0.5054 0.105 Uiso 0.4 1 calc R . P H 2
H45B H 0.1640 1.1307 0.4051 0.105 Uiso 0.4 1 calc R . P H 2
C46 C 0.0033(17) 1.0828(14) 0.4040(13) 0.073(5) Uani 0.4 1 d . U P H 2
H46A H -0.0131 1.1275 0.3665 0.088 Uiso 0.4 1 calc R . P H 2
H46B H -0.0274 1.0991 0.4530 0.088 Uiso 0.4 1 calc R . P H 2
C47 C -0.0528(18) 0.9664(15) 0.3450(13) 0.093(5) Uani 0.4 1 d . U P H 2
H47A H -0.1255 0.9343 0.3524 0.111 Uiso 0.4 1 calc R . P H 2
H47B H -0.0695 0.9563 0.2796 0.111 Uiso 0.4 1 calc R . P H 2
C55 C -0.0387(18) 0.4948(15) 0.1075(15) 0.097(6) Uani 0.35 1 d . U P G 2
H55A H -0.0237 0.5231 0.0606 0.116 Uiso 0.35 1 calc R . P G 2
H55B H -0.1152 0.4968 0.1081 0.116 Uiso 0.35 1 calc R . P G 2
C1 C 0.4313(3) 1.4223(3) 0.2617(2) 0.0311(8) Uani 1 1 d . . . . .
C2 C 0.3983(3) 1.4155(3) 0.1695(2) 0.0389(9) Uani 1 1 d . . . . .
H2 H 0.3699 1.3478 0.1231 0.047 Uiso 1 1 calc R . . . .
C3 C 0.4058(3) 1.5044(3) 0.1445(2) 0.0411(9) Uani 1 1 d . . . . .
H3 H 0.3843 1.4967 0.0817 0.049 Uiso 1 1 calc R . . . .
C4 C 0.4445(3) 1.6048(3) 0.2100(2) 0.0393(9) Uani 1 1 d . . . . .
H4 H 0.4493 1.6656 0.1925 0.047 Uiso 1 1 calc R . . . .
C5 C 0.4757(3) 1.6147(3) 0.3012(2) 0.0340(8) Uani 1 1 d . . . . .
H5 H 0.5030 1.6828 0.3469 0.041 Uiso 1 1 calc R . . . .
C6 C 0.4674(3) 1.5251(3) 0.3265(2) 0.0291(7) Uani 1 1 d . . . . .
C7 C 0.4919(3) 1.5240(2) 0.4204(2) 0.0261(7) Uani 1 1 d . . . . .
C8 C 0.4979(3) 1.4160(3) 0.4187(2) 0.0280(7) Uani 1 1 d . . . . .
H8 H 0.5790 1.4240 0.4226 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5025(3) 1.4008(3) 0.5076(2) 0.0285(7) Uani 1 1 d . . . . .
H9 H 0.5014 1.3337 0.5125 0.034 Uiso 1 1 calc R . . . .
C10 C 0.2748(3) 1.2676(3) 0.2658(2) 0.0294(7) Uani 1 1 d . . . . .
C11 C 0.2220(3) 1.1841(3) 0.1797(2) 0.0341(8) Uani 1 1 d . . . . .
C12 C 0.1020(3) 1.1323(3) 0.1393(2) 0.0357(8) Uani 1 1 d . . . . .
H12 H 0.0710 1.0761 0.0822 0.043 Uiso 1 1 calc R . . . .
C13 C 0.0268(3) 1.1597(3) 0.1792(3) 0.0394(9) Uani 1 1 d . . . . .
C14 C 0.0777(3) 1.2424(3) 0.2637(2) 0.0365(8) Uani 1 1 d . . . . .
H14 H 0.0291 1.2632 0.2937 0.044 Uiso 1 1 calc R . . . .
C15 C 0.1967(3) 1.2956(3) 0.3056(2) 0.0310(8) Uani 1 1 d . . . . .
C16 C 0.2889(4) 1.1413(3) 0.1253(2) 0.0411(9) Uani 1 1 d . . . . .
H16A H 0.3599 1.1980 0.1379 0.062 Uiso 1 1 calc GR . . . .
H16B H 0.2410 1.1148 0.0599 0.062 Uiso 1 1 calc GR . . . .
H16C H 0.3090 1.0835 0.1428 0.062 Uiso 1 1 calc GR . . . .
C17 C -0.1027(4) 1.1039(4) 0.1344(3) 0.0564(12) Uani 1 1 d . . . . .
H17A H -0.1236 1.0653 0.0694 0.085 Uiso 1 1 calc GR . . . .
H17B H -0.1424 1.1562 0.1407 0.085 Uiso 1 1 calc GR . . . .
H17C H -0.1261 1.0539 0.1640 0.085 Uiso 1 1 calc GR . . . .
C18 C 0.2361(3) 1.3840(3) 0.3954(2) 0.0404(9) Uani 1 1 d . . . . .
H18A H 0.2869 1.3677 0.4439 0.061 Uiso 1 1 calc GR . . . .
H18B H 0.1685 1.3917 0.4093 0.061 Uiso 1 1 calc GR . . . .
H18C H 0.2785 1.4503 0.3913 0.061 Uiso 1 1 calc GR . . . .
C19 C 0.4873(3) 1.2423(3) 0.2995(2) 0.0347(8) Uani 1 1 d . . . . .
C20 C 0.5836(4) 1.2519(3) 0.2718(2) 0.0451(10) Uani 1 1 d . . . . .
C21 C 0.6373(4) 1.1747(4) 0.2662(3) 0.0601(13) Uani 1 1 d . . . . .
H21 H 0.7002 1.1832 0.2460 0.072 Uiso 1 1 calc R . . . .
C22 C 0.6020(5) 1.0863(4) 0.2891(3) 0.0675(15) Uani 1 1 d . . . . .
C23 C 0.5146(4) 1.0795(3) 0.3207(3) 0.0556(12) Uani 1 1 d . . . . .
H23 H 0.4913 1.0212 0.3395 0.067 Uiso 1 1 calc R . . . .
C24 C 0.4570(3) 1.1537(3) 0.3270(2) 0.0409(9) Uani 1 1 d . . . . .
C25 C 0.3626(4) 1.1339(3) 0.3646(3) 0.0459(10) Uani 1 1 d . . . . .
H25A H 0.3584 1.2017 0.3976 0.069 Uiso 1 1 calc GR . . . .
H25B H 0.3801 1.0950 0.4065 0.069 Uiso 1 1 calc GR . . . .
H25C H 0.2882 1.0920 0.3141 0.069 Uiso 1 1 calc GR . . . .
C26 C 0.6635(7) 1.0044(6) 0.2844(5) 0.105(2) Uani 1 1 d . . . . .
H26A H 0.6518 0.9689 0.2206 0.157 Uiso 1 1 calc GR . . . .
H26B H 0.6318 0.9519 0.3090 0.157 Uiso 1 1 calc GR . . . .
H26C H 0.7466 1.0398 0.3206 0.157 Uiso 1 1 calc GR . . . .
C27 C 0.6334(4) 1.3461(4) 0.2485(3) 0.0591(12) Uani 1 1 d . . . . .
H27A H 0.5811 1.3412 0.1889 0.089 Uiso 1 1 calc GR . . . .
H27B H 0.7092 1.3474 0.2460 0.089 Uiso 1 1 calc GR . . . .
H27C H 0.6425 1.4112 0.2954 0.089 Uiso 1 1 calc GR . . . .
B1 B 0.4189(4) 1.3296(3) 0.3094(2) 0.0293(8) Uani 1 1 d . . . . .
O8 O -0.3269(7) 0.2013(7) -0.0164(7) 0.186(3) Uani 1 1 d . . . . .
C40 C -0.3635(9) 0.2872(7) -0.0016(6) 0.119(3) Uani 1 1 d . . . . .
H40A H -0.3422 0.3296 -0.0384 0.143 Uiso 1 1 calc R . . . .
H40B H -0.3251 0.3326 0.0637 0.143 Uiso 1 1 calc R . . . .
C41 C -0.4908(10) 0.2513(11) -0.0276(7) 0.149(4) Uani 1 1 d . . . . .
H41A H -0.5324 0.2423 -0.0921 0.179 Uiso 1 1 calc R . . . .
H41B H -0.5151 0.2999 0.0129 0.179 Uiso 1 1 calc R . . . .
C42 C -0.5081(9) 0.1415(10) -0.0120(6) 0.142(4) Uani 1 1 d . . . . .
H42A H -0.5083 0.1485 0.0498 0.170 Uiso 1 1 calc R . . . .
H42B H -0.5814 0.0872 -0.0582 0.170 Uiso 1 1 calc R . . . .
C43 C -0.4088(9) 0.1153(9) -0.0223(8) 0.142(3) Uani 1 1 d . . . . .
H43A H -0.3759 0.0875 0.0260 0.171 Uiso 1 1 calc R . . . .
H43B H -0.4336 0.0591 -0.0823 0.171 Uiso 1 1 calc R . . . .
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'
K K 0.2009 0.2494 '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'
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
O1 K1 O5 119.63(10) .
O2 K1 O1 60.26(11) .
O2 K1 O3 60.52(11) .
O2 K1 O5 179.23(9) .
O3 K1 O1 119.39(11) .
O3 K1 O5 119.41(10) .
O4 K1 O1 179.89(11) .
O4 K1 O2 119.82(11) .
O4 K1 O3 60.67(10) .
O4 K1 O5 60.29(10) .
O6 K1 O1 61.10(10) .
O6 K1 O2 119.85(11) .
O6 K1 O3 179.35(11) .
O6 K1 O4 118.84(10) .
O6 K1 O5 60.23(10) .
O7 K1 O1 85.38(11) .
O7 K1 O2 91.04(11) .
O7 K1 O3 83.90(11) .
O7 K1 O4 94.55(11) .
O7 K1 O5 88.20(10) .
O7 K1 O6 96.60(11) .
O10 K1 O1 96.7(2) .
O10 K1 O2 98.3(3) .
O10 K1 O3 103.2(2) .
O10 K1 O4 83.4(2) .
O10 K1 O5 82.5(3) .
O10 K1 O6 76.2(2) .
O10 K1 O7 170.2(3) .
O9 K1 O1 89.3(3) .
O9 K1 O2 82.6(2) .
O9 K1 O3 95.0(3) .
O9 K1 O4 90.8(3) .
O9 K1 O5 98.2(2) .
O9 K1 O6 84.5(3) .
O9 K1 O7 173.2(2) .
C28 O1 K1 113.9(3) .
C28 O1 C39 111.9(4) .
C39 O1 K1 110.7(3) .
C29 O2 K1 115.4(3) .
C30 O2 K1 115.3(3) .
C30 O2 C29 112.7(4) .
C31 O3 K1 114.1(3) .
C32 O3 K1 113.2(3) .
C32 O3 C31 112.1(4) .
C33 O4 K1 114.4(3) .
C33 O4 C34 111.8(4) .
C34 O4 K1 114.5(3) .
C35 O5 K1 114.1(3) .
C35 O5 C36 112.3(4) .
C36 O5 K1 113.8(3) .
C37 O6 K1 116.6(3) .
C38 O6 K1 116.0(3) .
C38 O6 C37 113.8(4) .
C44 O7 K1 108.9(3) .
C44 O7 C50 97.8(6) .
C44 O7 C47 125.9(9) .
C50 O7 K1 126.9(4) .
C47 O7 K1 122.2(7) .
O1 C28 C29 111.0(4) .
O2 C29 C28 109.2(4) .
O2 C30 C31 109.2(4) .
O3 C31 C30 110.3(4) .
O3 C32 C33 108.5(4) .
O4 C33 C32 110.9(4) .
O4 C34 C35 108.9(4) .
O5 C35 C34 110.5(4) .
O5 C36 C37 110.0(4) .
O6 C37 C36 109.9(4) .
O6 C38 C39 111.0(5) .
O1 C39 C38 109.9(4) .
O7 C44 C48 112.5(7) .
O7 C44 C45 90.8(9) .
C52 C51 O9 101.7(6) .
O10 C51 C52 114.0(7) .
C51 C52 C53 103.5(5) .
C52 C53 C54 102.2(7) .
C52 C53 C55 96.5(10) .
C51 O10 K1 129.4(7) .
C51 O10 C54 105.7(9) .
C54 O10 K1 121.2(8) .
C44 C48 C49 98.7(8) .
C50 C49 C48 104.6(9) .
O7 C50 C49 107.3(8) .
O10 C54 C53 107.7(10) .
C51 O9 K1 125.2(7) .
C55 O9 K1 121.9(10) .
C55 O9 C51 113.0(11) .
C46 C45 C44 107.9(15) .
C45 C46 C47 107.1(16) .
O7 C47 C46 102.6(14) .
O9 C55 C53 106.3(13) .
C2 C1 C6 115.7(3) .
C2 C1 B1 131.7(3) .
C6 C1 B1 112.0(3) .
C3 C2 C1 122.0(3) .
C2 C3 C4 120.9(3) .
C5 C4 C3 118.9(3) .
C4 C5 C6 120.3(3) .
C1 C6 C7 112.1(3) .
C5 C6 C1 122.2(3) .
C5 C6 C7 125.7(3) .
C6 C7 C8 107.3(3) .
C9 C7 C6 127.3(3) 2_686
C9 C7 C8 125.1(3) 2_686
C7 C8 B1 107.4(3) .
C9 C8 C7 111.2(3) .
C9 C8 B1 129.1(3) .
C7 C9 C8 123.6(3) 2_686
C11 C10 B1 119.8(3) .
C15 C10 C11 114.9(3) .
C15 C10 B1 125.2(3) .
C10 C11 C16 123.8(3) .
C12 C11 C10 121.8(3) .
C12 C11 C16 114.4(3) .
C13 C12 C11 122.7(3) .
C12 C13 C14 116.0(3) .
C12 C13 C17 122.1(4) .
C14 C13 C17 121.9(4) .
C15 C14 C13 122.7(4) .
C10 C15 C18 122.7(3) .
C14 C15 C10 121.8(3) .
C14 C15 C18 115.5(3) .
C20 C19 B1 125.2(3) .
C24 C19 C20 114.9(4) .
C24 C19 B1 119.8(3) .
C19 C20 C27 121.7(4) .
C21 C20 C19 121.5(4) .
C21 C20 C27 116.8(4) .
C22 C21 C20 122.2(5) .
C21 C22 C26 121.3(6) .
C23 C22 C21 116.7(4) .
C23 C22 C26 121.9(6) .
C22 C23 C24 123.6(5) .
C19 C24 C25 122.8(3) .
C23 C24 C19 120.9(4) .
C23 C24 C25 116.2(4) .
C1 B1 C8 94.8(3) .
C1 B1 C10 102.1(3) .
C10 B1 C8 125.2(3) .
C19 B1 C1 122.7(3) .
C19 B1 C8 102.7(3) .
C19 B1 C10 110.4(3) .
C43 O8 C40 109.7(8) .
O8 C40 C41 109.8(9) .
C40 C41 C42 99.1(7) .
C43 C42 C41 103.0(8) .
O8 C43 C42 110.8(10) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.828(3) .
K1 O2 2.810(3) .
K1 O3 2.813(3) .
K1 O4 2.792(3) .
K1 O5 2.829(3) .
K1 O6 2.764(3) .
K1 O7 2.734(3) .
K1 O10 2.713(11) .
K1 O9 2.661(10) .
O1 C28 1.376(6) .
O1 C39 1.426(6) .
O2 C29 1.412(6) .
O2 C30 1.408(7) .
O3 C31 1.423(6) .
O3 C32 1.391(6) .
O4 C33 1.379(6) .
O4 C34 1.383(6) .
O5 C35 1.367(6) .
O5 C36 1.392(6) .
O6 C37 1.425(6) .
O6 C38 1.373(6) .
O7 C44 1.399(8) .
O7 C50 1.418(10) .
O7 C47 1.463(17) .
C28 C29 1.512(8) .
C30 C31 1.503(9) .
C32 C33 1.514(8) .
C34 C35 1.527(8) .
C36 C37 1.487(8) .
C38 C39 1.487(8) .
C44 C48 1.462(10) .
C44 C45 1.82(2) .
C51 C52 1.448(8) .
C51 O10 1.345(12) .
C51 O9 1.479(13) .
C52 C53 1.484(10) .
C53 C54 1.522(14) .
C53 C55 1.551(19) .
O10 C54 1.388(15) .
C48 C49 1.519(15) .
C49 C50 1.507(15) .
O9 C55 1.21(2) .
C45 C46 1.43(2) .
C46 C47 1.52(2) .
C1 C2 1.410(5) .
C1 C6 1.413(5) .
C1 B1 1.662(5) .
C2 C3 1.383(5) .
C3 C4 1.390(5) .
C4 C5 1.384(5) .
C5 C6 1.395(5) .
C6 C7 1.477(4) .
C7 C8 1.510(5) .
C7 C9 1.329(4) 2_686
C8 C9 1.504(4) .
C8 B1 1.710(5) .
C9 C7 1.329(4) 2_686
C10 C11 1.420(5) .
C10 C15 1.419(5) .
C10 B1 1.681(5) .
C11 C12 1.399(5) .
C11 C16 1.515(5) .
C12 C13 1.383(6) .
C13 C14 1.399(5) .
C13 C17 1.511(5) .
C14 C15 1.392(5) .
C15 C18 1.505(5) .
C19 C20 1.424(6) .
C19 C24 1.420(5) .
C19 B1 1.655(5) .
C20 C21 1.400(6) .
C20 C27 1.504(7) .
C21 C22 1.384(8) .
C22 C23 1.358(7) .
C22 C26 1.524(7) .
C23 C24 1.400(6) .
C24 C25 1.510(6) .
O8 C40 1.370(10) .
O8 C43 1.351(11) .
C40 C41 1.480(13) .
C41 C42 1.580(14) .
C42 C43 1.446(12) .
