#------------------------------------------------------------------------------
#$Date: 2019-11-17 07:18:36 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228624 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/94/1549474.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_1549474
loop_
_publ_author_name
'Chen, Chang-Hong'
'Gabbaï, François P'
_publ_section_title
;
 Large-bite diboranes for the μ(1,2) complexation of hydrazine and
 cyanide.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              6210
_journal_page_last               6218
_journal_paper_doi               10.1039/c8sc01877d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C21 H26 Cl2 K O6, C H2 Cl2, C49 H50 B2 N'
_chemical_formula_sum            'C71 H78 B2 Cl4 K N O6'
_chemical_formula_weight         1243.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-03-02 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.9484(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4096(14)
_cell_length_b                   23.693(2)
_cell_length_c                   19.0628(17)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.541
_cell_measurement_theta_min      2.201
_cell_volume                     6409.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            140726
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         2.074
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0797 before and 0.0572 after correction. The Ratio of minimum to maximum transmission is 0.9277. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         14800
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0785P)²+7.7626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10757
_reflns_number_total             14800
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc01877d2.cif
_cod_data_source_block           1CN
_cod_depositor_comments
'Adding full bibliography for 1549471--1549474.cif.'
_cod_database_code               1549474
_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.
;
_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. Uiso/Uaniso restraints and constraints
B2 \\sim B1 \\sim N2 \\sim C72: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
B2 \\sim B1 \\sim N1 \\sim C71: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(N1) = Uanis(N2)
Uanis(C71) = Uanis(C72)
3. Others
 Sof(N2)=Sof(C72)=1-FVAR(1)
 Sof(N1)=Sof(C71)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B), C65(H65A,H65B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B)
4.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54), C61(H61), C62(H62), C63(H63),
 C64(H64), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C15(H15),
 C17(H17), C24(H24), C26(H26), C33(H33), C35(H35), C42(H42), C44(H44)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
K1 K 0.14200(4) 0.39928(3) 0.05282(4) 0.02900(15) Uani 1 1 d . . . . .
Cl1 Cl 0.24750(6) 0.27866(3) 0.17120(4) 0.04079(19) Uani 1 1 d . . . . .
Cl2 Cl 0.25204(5) 0.18372(3) 0.07508(5) 0.0436(2) Uani 1 1 d . . . . .
O1 O 0.11412(13) 0.48107(8) 0.14499(11) 0.0278(4) Uani 1 1 d . . . . .
O2 O -0.02292(12) 0.41199(8) 0.07682(11) 0.0246(4) Uani 1 1 d . . . . .
O3 O 0.00111(13) 0.32206(8) -0.00995(11) 0.0246(4) Uani 1 1 d . . . . .
O4 O 0.17595(12) 0.30776(8) -0.02212(10) 0.0252(4) Uani 1 1 d . . . . .
O5 O 0.31700(12) 0.37225(8) 0.05651(10) 0.0238(4) Uani 1 1 d . . . . .
O6 O 0.29603(12) 0.46096(8) 0.14618(10) 0.0253(4) Uani 1 1 d . . . . .
C49 C 0.02515(18) 0.50274(12) 0.12769(15) 0.0240(5) Uani 1 1 d . . . . .
C50 C -0.04938(18) 0.46498(11) 0.09041(15) 0.0232(5) Uani 1 1 d . . . . .
C51 C -0.14151(19) 0.48222(12) 0.07216(15) 0.0261(6) Uani 1 1 d . . . . .
H51 H -0.1920 0.4571 0.0464 0.031 Uiso 1 1 calc R . . . .
C52 C -0.1602(2) 0.53604(12) 0.09138(16) 0.0288(6) Uani 1 1 d . . . . .
H52 H -0.2234 0.5476 0.0794 0.035 Uiso 1 1 calc R . . . .
C53 C -0.0872(2) 0.57272(12) 0.12782(17) 0.0300(6) Uani 1 1 d . . . . .
H53 H -0.1002 0.6095 0.1411 0.036 Uiso 1 1 calc R . . . .
C54 C 0.0058(2) 0.55635(12) 0.14535(17) 0.0294(6) Uani 1 1 d . . . . .
H54 H 0.0557 0.5822 0.1695 0.035 Uiso 1 1 calc R . . . .
C55 C -0.09775(18) 0.37307(12) 0.03825(16) 0.0265(6) Uani 1 1 d . . . . .
H55A H -0.1357 0.3869 -0.0138 0.032 Uiso 1 1 calc R . . . .
H55B H -0.1397 0.3694 0.0663 0.032 Uiso 1 1 calc R . . . .
C56 C -0.0546(2) 0.31709(12) 0.03439(18) 0.0279(6) Uani 1 1 d . . . . .
H56A H -0.105(2) 0.2896(14) 0.0132(18) 0.029(8) Uiso 1 1 d . . . . .
H56B H -0.020(2) 0.3025(14) 0.0818(19) 0.028(8) Uiso 1 1 d . . . . .
C57 C 0.03391(19) 0.26815(11) -0.02226(17) 0.0271(6) Uani 1 1 d . . . . .
H57A H -0.0205 0.2437 -0.0507 0.032 Uiso 1 1 calc R . . . .
H57B H 0.0702 0.2500 0.0274 0.032 Uiso 1 1 calc R . . . .
C58 C 0.09505(18) 0.27446(12) -0.06633(16) 0.0270(6) Uani 1 1 d . . . . .
H58A H 0.1154 0.2369 -0.0768 0.032 Uiso 1 1 calc R . . . .
H58B H 0.0595 0.2933 -0.1156 0.032 Uiso 1 1 calc R . . . .
C59 C 0.24699(18) 0.31209(11) -0.04893(15) 0.0238(5) Uani 1 1 d . . . . .
C60 C 0.32304(18) 0.34701(11) -0.00648(14) 0.0226(5) Uani 1 1 d . . . . .
C61 C 0.39773(18) 0.35406(12) -0.02900(15) 0.0253(5) Uani 1 1 d . . . . .
H61 H 0.4487 0.3782 -0.0010 0.030 Uiso 1 1 calc R . . . .
C62 C 0.3976(2) 0.32566(13) -0.09267(16) 0.0308(6) Uani 1 1 d . . . . .
H62 H 0.4491 0.3301 -0.1078 0.037 Uiso 1 1 calc R . . . .
C63 C 0.3239(2) 0.29119(14) -0.13394(17) 0.0340(7) Uani 1 1 d . . . . .
H63 H 0.3245 0.2719 -0.1775 0.041 Uiso 1 1 calc R . . . .
C64 C 0.2481(2) 0.28434(13) -0.11218(16) 0.0318(6) Uani 1 1 d . . . . .
H64 H 0.1970 0.2605 -0.1410 0.038 Uiso 1 1 calc R . . . .
C65 C 0.39499(18) 0.40696(12) 0.10224(15) 0.0244(5) Uani 1 1 d . . . . .
H65A H 0.4001 0.4402 0.0727 0.029 Uiso 1 1 calc R . . . .
H65B H 0.4545 0.3853 0.1181 0.029 Uiso 1 1 calc R . . . .
C66 C 0.37792(18) 0.42550(12) 0.17079(16) 0.0259(6) Uani 1 1 d . . . . .
H66A H 0.433(2) 0.4474(14) 0.2034(18) 0.032(8) Uiso 1 1 d . . . . .
H66B H 0.3667(19) 0.3924(13) 0.1997(16) 0.021(7) Uiso 1 1 d . . . . .
C67 C 0.28074(19) 0.48377(13) 0.20946(16) 0.0295(6) Uani 1 1 d . . . . .
H67A H 0.3351 0.5075 0.2404 0.035 Uiso 1 1 calc R . . . .
H67B H 0.2744 0.4528 0.2420 0.035 Uiso 1 1 calc R . . . .
C68 C 0.19270(19) 0.51861(12) 0.18077(18) 0.0309(6) Uani 1 1 d . . . . .
H68A H 0.1854 0.5389 0.2236 0.037 Uiso 1 1 calc R . . . .
H68B H 0.1958 0.5468 0.1435 0.037 Uiso 1 1 calc R . . . .
C69 C 0.3155(2) 0.24019(13) 0.13120(19) 0.0368(7) Uani 1 1 d . . . . .
H69A H 0.3359 0.2658 0.0995 0.044 Uiso 1 1 calc R . . . .
H69B H 0.3727 0.2255 0.1727 0.044 Uiso 1 1 calc R . . . .
Cl3 Cl 0.17824(6) 0.47411(4) 0.35050(5) 0.0455(2) Uani 1 1 d . . . . .
Cl4 Cl 0.18439(7) 0.36117(4) 0.29112(8) 0.0656(3) Uani 1 1 d . . . . .
C70 C 0.1123(2) 0.41460(14) 0.3039(2) 0.0423(8) Uani 1 1 d . . . . .
H70A H 0.0650 0.4261 0.2536 0.051 Uiso 1 1 calc R . . . .
H70B H 0.0780 0.3995 0.3343 0.051 Uiso 1 1 calc R . . . .
C1 C 0.29775(16) 0.79130(10) 0.40284(13) 0.0176(5) Uani 1 1 d . . . . .
C2 C 0.29937(17) 0.77354(11) 0.47520(14) 0.0207(5) Uani 1 1 d . . . . .
H2 H 0.2805 0.7360 0.4795 0.025 Uiso 1 1 calc R . . . .
C3 C 0.32653(18) 0.80752(12) 0.53918(14) 0.0230(5) Uani 1 1 d . . . . .
H3 H 0.3267 0.7924 0.5854 0.028 Uiso 1 1 calc R . . . .
C4 C 0.35393(17) 0.86403(12) 0.53737(14) 0.0230(5) Uani 1 1 d . . . . .
H4 H 0.3731 0.8878 0.5809 0.028 Uiso 1 1 calc R . . . .
C5 C 0.35092(16) 0.88223(11) 0.46848(14) 0.0189(5) Uani 1 1 d . . . . .
C6 C 0.32247(16) 0.84711(10) 0.40265(13) 0.0175(5) Uani 1 1 d . . . . .
C7 C 0.34011(16) 0.89696(10) 0.35784(14) 0.0179(5) Uani 1 1 d . . . . .
C8 C 0.33562(16) 0.91788(10) 0.28896(13) 0.0177(5) Uani 1 1 d . . . . .
C9 C 0.37277(17) 0.97395(10) 0.29530(15) 0.0209(5) Uani 1 1 d . . . . .
H9 H 0.3782 0.9900 0.2515 0.025 Uiso 1 1 calc R . . . .
C10 C 0.40114(17) 1.00606(11) 0.36051(15) 0.0229(5) Uani 1 1 d . . . . .
H10 H 0.4235 1.0433 0.3597 0.027 Uiso 1 1 calc R . . . .
C11 C 0.39780(17) 0.98501(11) 0.42851(15) 0.0227(5) Uani 1 1 d . . . . .
H11 H 0.4141 1.0073 0.4732 0.027 Uiso 1 1 calc R . . . .
C12 C 0.36928(16) 0.92995(11) 0.42545(14) 0.0189(5) Uani 1 1 d . . . . .
C13 C 0.33941(17) 0.70255(10) 0.31914(14) 0.0180(5) Uani 1 1 d . . . . .
C14 C 0.30774(18) 0.67088(10) 0.25075(14) 0.0205(5) Uani 1 1 d . . . . .
C15 C 0.36644(19) 0.63157(11) 0.23696(15) 0.0241(5) Uani 1 1 d . . . . .
H15 H 0.3431 0.6108 0.1907 0.029 Uiso 1 1 calc R . . . .
C16 C 0.4574(2) 0.62182(11) 0.28818(16) 0.0266(6) Uani 1 1 d . . . . .
C17 C 0.48973(18) 0.65359(11) 0.35446(15) 0.0245(5) Uani 1 1 d . . . . .
H17 H 0.5522 0.6478 0.3905 0.029 Uiso 1 1 calc R . . . .
C18 C 0.43357(18) 0.69385(11) 0.37005(14) 0.0211(5) Uani 1 1 d . . . . .
C19 C 0.20997(19) 0.67680(11) 0.18888(15) 0.0248(5) Uani 1 1 d . . . . .
H19A H 0.1631 0.6634 0.2080 0.037 Uiso 1 1 calc GR . . . .
H19B H 0.2057 0.6543 0.1445 0.037 Uiso 1 1 calc GR . . . .
H19C H 0.1979 0.7165 0.1740 0.037 Uiso 1 1 calc GR . . . .
C20 C 0.5190(2) 0.57802(14) 0.2735(2) 0.0395(7) Uani 1 1 d . . . . .
H20A H 0.5276 0.5462 0.3083 0.059 Uiso 1 1 calc GR . . . .
H20B H 0.5805 0.5946 0.2817 0.059 Uiso 1 1 calc GR . . . .
H20C H 0.4890 0.5647 0.2207 0.059 Uiso 1 1 calc GR . . . .
C21 C 0.47952(19) 0.72585(12) 0.44405(16) 0.0286(6) Uani 1 1 d . . . . .
H21A H 0.4697 0.7664 0.4343 0.043 Uiso 1 1 calc GR . . . .
H21B H 0.5472 0.7178 0.4660 0.043 Uiso 1 1 calc GR . . . .
H21C H 0.4514 0.7141 0.4798 0.043 Uiso 1 1 calc GR . . . .
C22 C 0.16466(17) 0.71854(10) 0.32380(13) 0.0186(5) Uani 1 1 d . . . . .
C23 C 0.15995(18) 0.66324(11) 0.35034(14) 0.0202(5) Uani 1 1 d . . . . .
C24 C 0.07345(18) 0.63927(11) 0.34119(15) 0.0235(5) Uani 1 1 d . . . . .
H24 H 0.0724 0.6017 0.3583 0.028 Uiso 1 1 calc R . . . .
C25 C -0.01096(18) 0.66821(12) 0.30813(15) 0.0248(5) Uani 1 1 d . . . . .
C26 C -0.00633(18) 0.72333(12) 0.28575(15) 0.0244(5) Uani 1 1 d . . . . .
H26 H -0.0628 0.7447 0.2649 0.029 Uiso 1 1 calc R . . . .
C27 C 0.07865(18) 0.74847(11) 0.29284(14) 0.0227(5) Uani 1 1 d . . . . .
C28 C 0.24595(19) 0.62664(11) 0.39089(15) 0.0241(5) Uani 1 1 d . . . . .
H28A H 0.2648 0.6080 0.3531 0.036 Uiso 1 1 calc GR . . . .
H28B H 0.2307 0.5980 0.4214 0.036 Uiso 1 1 calc GR . . . .
H28C H 0.2978 0.6503 0.4243 0.036 Uiso 1 1 calc GR . . . .
C29 C -0.10343(19) 0.64190(14) 0.30032(17) 0.0326(6) Uani 1 1 d . . . . .
H29A H -0.0945 0.6013 0.3107 0.049 Uiso 1 1 calc GR . . . .
H29B H -0.1500 0.6478 0.2484 0.049 Uiso 1 1 calc GR . . . .
H29C H -0.1258 0.6595 0.3367 0.049 Uiso 1 1 calc GR . . . .
C30 C 0.07325(19) 0.80931(12) 0.26694(17) 0.0298(6) Uani 1 1 d . . . . .
H30A H 0.1276 0.8302 0.3022 0.045 Uiso 1 1 calc GR . . . .
H30B H 0.0150 0.8265 0.2662 0.045 Uiso 1 1 calc GR . . . .
H30C H 0.0736 0.8106 0.2157 0.045 Uiso 1 1 calc GR . . . .
C31 C 0.36859(17) 0.89013(10) 0.16624(14) 0.0185(5) Uani 1 1 d . . . . .
C32 C 0.36656(18) 0.93486(11) 0.11585(14) 0.0224(5) Uani 1 1 d . . . . .
C33 C 0.43394(19) 0.93820(12) 0.08417(15) 0.0269(6) Uani 1 1 d . . . . .
H33 H 0.4314 0.9691 0.0516 0.032 Uiso 1 1 calc R . . . .
C34 C 0.50429(19) 0.89850(13) 0.09808(15) 0.0276(6) Uani 1 1 d . . . . .
C35 C 0.50767(18) 0.85560(12) 0.14730(15) 0.0258(6) Uani 1 1 d . . . . .
H35 H 0.5558 0.8279 0.1584 0.031 Uiso 1 1 calc R . . . .
C36 C 0.44291(17) 0.85108(11) 0.18167(14) 0.0216(5) Uani 1 1 d . . . . .
C37 C 0.29081(19) 0.97940(12) 0.09008(16) 0.0279(6) Uani 1 1 d . . . . .
H37A H 0.2349 0.9643 0.0487 0.042 Uiso 1 1 calc GR . . . .
H37B H 0.3140 1.0125 0.0719 0.042 Uiso 1 1 calc GR . . . .
H37C H 0.2742 0.9903 0.1329 0.042 Uiso 1 1 calc GR . . . .
C38 C 0.5744(2) 0.90326(16) 0.0609(2) 0.0413(8) Uani 1 1 d . . . . .
H38A H 0.5406 0.9062 0.0055 0.062 Uiso 1 1 calc GR . . . .
H38B H 0.6148 0.8697 0.0730 0.062 Uiso 1 1 calc GR . . . .
H38C H 0.6134 0.9370 0.0799 0.062 Uiso 1 1 calc GR . . . .
C39 C 0.4570(2) 0.80202(13) 0.23605(17) 0.0308(6) Uani 1 1 d . . . . .
H39A H 0.4513 0.8154 0.2827 0.046 Uiso 1 1 calc GR . . . .
H39B H 0.5198 0.7858 0.2487 0.046 Uiso 1 1 calc GR . . . .
H39C H 0.4090 0.7732 0.2119 0.046 Uiso 1 1 calc GR . . . .
C40 C 0.18125(16) 0.90233(10) 0.14861(13) 0.0172(5) Uani 1 1 d . . . . .
C41 C 0.12135(18) 0.94149(10) 0.16356(15) 0.0211(5) Uani 1 1 d . . . . .
C42 C 0.03083(18) 0.95132(11) 0.10929(16) 0.0255(6) Uani 1 1 d . . . . .
H42 H -0.0068 0.9791 0.1199 0.031 Uiso 1 1 calc R . . . .
C43 C -0.00683(18) 0.92258(11) 0.04091(15) 0.0254(5) Uani 1 1 d . . . . .
C44 C 0.04965(18) 0.88234(11) 0.02775(15) 0.0231(5) Uani 1 1 d . . . . .
H44 H 0.0252 0.8610 -0.0180 0.028 Uiso 1 1 calc R . . . .
C45 C 0.14123(17) 0.87189(10) 0.07924(14) 0.0192(5) Uani 1 1 d . . . . .
C46 C 0.1480(2) 0.97509(13) 0.23613(16) 0.0314(6) Uani 1 1 d . . . . .
H46A H 0.1704 0.9494 0.2799 0.047 Uiso 1 1 calc GR . . . .
H46B H 0.0928 0.9958 0.2358 0.047 Uiso 1 1 calc GR . . . .
H46C H 0.1981 1.0018 0.2399 0.047 Uiso 1 1 calc GR . . . .
C47 C -0.1045(2) 0.93515(14) -0.01573(18) 0.0361(7) Uani 1 1 d . . . . .
H47A H -0.1496 0.9303 0.0086 0.054 Uiso 1 1 calc GR . . . .
H47B H -0.1205 0.9092 -0.0590 0.054 Uiso 1 1 calc GR . . . .
H47C H -0.1073 0.9741 -0.0337 0.054 Uiso 1 1 calc GR . . . .
C48 C 0.19505(18) 0.82754(11) 0.05629(14) 0.0233(5) Uani 1 1 d . . . . .
H48A H 0.2514 0.8445 0.0530 0.035 Uiso 1 1 calc GR . . . .
H48B H 0.1550 0.8120 0.0065 0.035 Uiso 1 1 calc GR . . . .
H48C H 0.2139 0.7973 0.0943 0.035 Uiso 1 1 calc GR . . . .
B2 B 0.29104(19) 0.88666(11) 0.20561(15) 0.0171(5) Uani 1 1 d . U . . .
B1 B 0.26444(19) 0.74742(12) 0.33100(15) 0.0176(5) Uani 1 1 d . U . . .
N1 N 0.2753(17) 0.8238(11) 0.2317(13) 0.016(3) Uani 0.47(3) 1 d . U P A 1
C71 C 0.257(2) 0.7917(14) 0.2641(13) 0.020(4) Uani 0.47(3) 1 d . U P A 1
N2 N 0.2529(13) 0.7889(8) 0.2633(10) 0.016(3) Uani 0.53(3) 1 d . U P A 2
C72 C 0.2732(19) 0.8273(13) 0.2306(12) 0.020(4) Uani 0.53(3) 1 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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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
_geom_angle_site_symmetry_3
O1 K1 Cl1 107.57(5) . .
O1 K1 O2 55.78(5) . .
O1 K1 O6 61.75(5) . .
O1 K1 C52 107.06(7) . 3_565
O1 K1 C53 119.11(7) . 3_565
O2 K1 Cl1 101.62(5) . .
O2 K1 C52 118.39(7) . 3_565
O2 K1 C53 105.93(7) . 3_565
O3 K1 Cl1 80.27(4) . .
O3 K1 O1 117.04(6) . .
O3 K1 O2 61.41(5) . .
O3 K1 O4 61.66(5) . .
O3 K1 O5 117.37(6) . .
O3 K1 O6 166.40(6) . .
O3 K1 C52 105.12(7) . 3_565
O3 K1 C53 80.80(7) . 3_565
O4 K1 Cl1 64.61(4) . .
O4 K1 O1 172.06(6) . .
O4 K1 O2 122.89(6) . .
O4 K1 O6 117.43(6) . .
O4 K1 C52 80.58(7) . 3_565
O4 K1 C53 68.78(7) . 3_565
O5 K1 Cl1 66.49(4) . .
O5 K1 O1 122.87(6) . .
O5 K1 O2 167.62(6) . .
O5 K1 O4 56.42(5) . .
O5 K1 O6 61.23(5) . .
O5 K1 C52 73.99(6) . 3_565
O5 K1 C53 85.55(6) . 3_565
O6 K1 Cl1 87.23(4) . .
O6 K1 O2 116.69(6) . .
O6 K1 C52 87.69(7) . 3_565
O6 K1 C53 111.98(7) . 3_565
C52 K1 Cl1 137.27(5) 3_565 .
C52 K1 C53 24.33(7) 3_565 3_565
C53 K1 Cl1 133.27(5) 3_565 .
C69 Cl1 K1 109.65(11) . .
C49 O1 K1 119.78(15) . .
C49 O1 C68 117.2(2) . .
C68 O1 K1 115.08(16) . .
C50 O2 K1 119.27(15) . .
C50 O2 C55 116.4(2) . .
C55 O2 K1 116.83(15) . .
C56 O3 K1 110.81(15) . .
C56 O3 C57 111.0(2) . .
C57 O3 K1 113.56(14) . .
C58 O4 K1 116.05(15) . .
C59 O4 K1 118.13(15) . .
C59 O4 C58 117.1(2) . .
C60 O5 K1 118.60(14) . .
C60 O5 C65 116.9(2) . .
C65 O5 K1 117.57(15) . .
C66 O6 K1 109.03(15) . .
C67 O6 K1 111.23(15) . .
C67 O6 C66 111.1(2) . .
O1 C49 C50 115.0(2) . .
C54 C49 O1 125.2(2) . .
C54 C49 C50 119.8(2) . .
O2 C50 C49 115.5(2) . .
O2 C50 C51 124.9(2) . .
C51 C50 C49 119.5(2) . .
C50 C51 C52 120.2(3) . .
C51 C52 K1 96.59(17) . 3_565
C53 C52 K1 78.82(17) . 3_565
C53 C52 C51 120.0(3) . .
C52 C53 K1 76.85(17) . 3_565
C52 C53 C54 120.5(3) . .
C54 C53 K1 97.36(18) . 3_565
C49 C54 C53 120.0(3) . .
O2 C55 C56 108.1(2) . .
O3 C56 C55 109.7(2) . .
O3 C57 C58 110.1(2) . .
O4 C58 C57 108.5(2) . .
O4 C59 C60 115.7(2) . .
C64 C59 O4 124.7(2) . .
C64 C59 C60 119.5(2) . .
O5 C60 C59 115.7(2) . .
O5 C60 C61 124.4(2) . .
C61 C60 C59 120.0(2) . .
C60 C61 C62 119.6(3) . .
C63 C62 C61 120.6(3) . .
C62 C63 C64 120.1(3) . .
C59 C64 C63 120.1(3) . .
O5 C65 C66 107.9(2) . .
O6 C66 C65 108.6(2) . .
O6 C67 C68 109.0(2) . .
O1 C68 C67 107.9(2) . .
Cl2 C69 Cl1 111.89(17) . .
Cl3 C70 Cl4 111.91(18) . .
C2 C1 B1 120.1(2) . .
C6 C1 C2 112.6(2) . .
C6 C1 B1 127.3(2) . .
C3 C2 C1 124.3(2) . .
C2 C3 C4 121.5(2) . .
C5 C4 C3 115.2(2) . .
C4 C5 C6 123.1(2) . .
C4 C5 C12 145.9(2) . .
C6 C5 C12 91.00(19) . .
C1 C6 C5 123.3(2) . .
C1 C6 C7 147.7(2) . .
C5 C6 C7 88.87(19) . .
C8 C7 C6 148.0(2) . .
C8 C7 C12 123.1(2) . .
C12 C7 C6 88.90(19) . .
C7 C8 C9 112.5(2) . .
C7 C8 B2 127.3(2) . .
C9 C8 B2 120.2(2) . .
C10 C9 C8 124.4(2) . .
C9 C10 C11 121.6(2) . .
C12 C11 C10 115.1(2) . .
C7 C12 C5 91.2(2) . .
C11 C12 C5 145.8(2) . .
C11 C12 C7 123.0(2) . .
C14 C13 B1 117.4(2) . .
C18 C13 C14 116.7(2) . .
C18 C13 B1 126.0(2) . .
C13 C14 C19 123.3(2) . .
C15 C14 C13 120.8(2) . .
C15 C14 C19 115.9(2) . .
C16 C15 C14 122.2(2) . .
C15 C16 C17 117.4(2) . .
C15 C16 C20 121.6(3) . .
C17 C16 C20 121.0(3) . .
C16 C17 C18 122.2(2) . .
C13 C18 C21 123.4(2) . .
C17 C18 C13 120.7(2) . .
C17 C18 C21 116.0(2) . .
C23 C22 B1 122.2(2) . .
C27 C22 C23 116.3(2) . .
C27 C22 B1 121.5(2) . .
C22 C23 C28 123.6(2) . .
C24 C23 C22 120.7(2) . .
C24 C23 C28 115.6(2) . .
C25 C24 C23 122.5(2) . .
C24 C25 C29 121.6(3) . .
C26 C25 C24 117.1(2) . .
C26 C25 C29 121.3(3) . .
C25 C26 C27 122.1(2) . .
C22 C27 C30 122.5(2) . .
C26 C27 C22 121.2(2) . .
C26 C27 C30 116.4(2) . .
C32 C31 B2 121.2(2) . .
C36 C31 C32 115.6(2) . .
C36 C31 B2 123.2(2) . .
C31 C32 C37 123.5(2) . .
C33 C32 C31 120.8(2) . .
C33 C32 C37 115.6(2) . .
C34 C33 C32 122.7(3) . .
C33 C34 C38 120.7(3) . .
C35 C34 C33 117.0(2) . .
C35 C34 C38 122.2(3) . .
C34 C35 C36 122.4(3) . .
C31 C36 C39 122.2(2) . .
C35 C36 C31 121.5(2) . .
C35 C36 C39 116.2(2) . .
C41 C40 C45 116.1(2) . .
C41 C40 B2 126.5(2) . .
C45 C40 B2 117.3(2) . .
C40 C41 C46 124.4(2) . .
C42 C41 C40 120.2(2) . .
C42 C41 C46 115.4(2) . .
C43 C42 C41 123.2(2) . .
C42 C43 C47 121.0(3) . .
C44 C43 C42 116.7(2) . .
C44 C43 C47 122.3(3) . .
C43 C44 C45 122.2(2) . .
C40 C45 C48 122.5(2) . .
C44 C45 C40 121.3(2) . .
C44 C45 C48 116.2(2) . .
C8 B2 C31 108.38(19) . .
C8 B2 C40 118.0(2) . .
C31 B2 C40 115.3(2) . .
N1 B2 C8 100.0(8) . .
N1 B2 C31 114.2(9) . .
N1 B2 C40 99.8(8) . .
C72 B2 C8 99.8(8) . .
C72 B2 C31 115.8(9) . .
C72 B2 C40 98.5(9) . .
C1 B1 C13 121.1(2) . .
C1 B1 C22 108.3(2) . .
C22 B1 C13 113.8(2) . .
C71 B1 C1 98.6(10) . .
C71 B1 C13 98.5(11) . .
C71 B1 C22 115.4(11) . .
N2 B1 C1 100.9(7) . .
N2 B1 C13 98.7(8) . .
N2 B1 C22 112.9(7) . .
C71 N1 B2 158(3) . .
N1 C71 B1 162(3) . .
C72 N2 B1 157.0(19) . .
N2 C72 B2 163(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 Cl1 3.6113(11) .
K1 O1 2.760(2) .
K1 O2 2.7687(19) .
K1 O3 2.7326(19) .
K1 O4 2.7567(19) .
K1 O5 2.7458(19) .
K1 O6 2.7645(19) .
K1 C52 3.253(3) 3_565
K1 C53 3.278(3) 3_565
Cl1 C69 1.770(3) .
Cl2 C69 1.754(3) .
O1 C49 1.378(3) .
O1 C68 1.442(3) .
O2 C50 1.375(3) .
O2 C55 1.435(3) .
O3 C56 1.426(3) .
O3 C57 1.426(3) .
O4 C58 1.438(3) .
O4 C59 1.381(3) .
O5 C60 1.377(3) .
O5 C65 1.437(3) .
O6 C66 1.434(3) .
O6 C67 1.423(3) .
C49 C50 1.410(4) .
C49 C54 1.376(4) .
C50 C51 1.385(4) .
C51 C52 1.388(4) .
C52 K1 3.253(3) 3_565
C52 C53 1.376(4) .
C53 K1 3.278(3) 3_565
C53 C54 1.393(4) .
C55 C56 1.498(4) .
C57 C58 1.494(4) .
C59 C60 1.405(4) .
C59 C64 1.379(4) .
C60 C61 1.386(4) .
C61 C62 1.387(4) .
C62 C63 1.371(4) .
C63 C64 1.393(4) .
C65 C66 1.496(4) .
C67 C68 1.497(4) .
Cl3 C70 1.762(3) .
Cl4 C70 1.763(3) .
C1 C2 1.433(3) .
C1 C6 1.376(3) .
C1 B1 1.635(4) .
C2 C3 1.383(4) .
C3 C4 1.408(4) .
C4 C5 1.366(4) .
C5 C6 1.425(3) .
C5 C12 1.487(4) .
C6 C7 1.543(3) .
C7 C8 1.380(3) .
C7 C12 1.422(3) .
C8 C9 1.433(3) .
C8 B2 1.641(4) .
C9 C10 1.375(4) .
C10 C11 1.408(4) .
C11 C12 1.371(4) .
C13 C14 1.416(3) .
C13 C18 1.411(3) .
C13 B1 1.649(4) .
C14 C15 1.393(4) .
C14 C19 1.515(3) .
C15 C16 1.379(4) .
C16 C17 1.386(4) .
C16 C20 1.505(4) .
C17 C18 1.395(4) .
C18 C21 1.512(4) .
C22 C23 1.416(4) .
C22 C27 1.413(3) .
C22 B1 1.639(4) .
C23 C24 1.396(4) .
C23 C28 1.519(4) .
C24 C25 1.386(4) .
C25 C26 1.384(4) .
C25 C29 1.508(4) .
C26 C27 1.396(4) .
C27 C30 1.516(4) .
C31 C32 1.423(4) .
C31 C36 1.411(3) .
C31 B2 1.643(4) .
C32 C33 1.392(4) .
C32 C37 1.507(4) .
C33 C34 1.381(4) .
C34 C35 1.370(4) .
C34 C38 1.511(4) .
C35 C36 1.395(4) .
C36 C39 1.516(4) .
C40 C41 1.414(3) .
C40 C45 1.419(3) .
C40 B2 1.657(3) .
C41 C42 1.395(4) .
C41 C46 1.508(4) .
C42 C43 1.382(4) .
C43 C44 1.378(4) .
C43 C47 1.501(4) .
C44 C45 1.391(3) .
C45 C48 1.505(4) .
B2 N1 1.62(3) .
B2 C72 1.54(4) .
B1 C71 1.62(3) .
B1 N2 1.58(2) .
N1 C71 1.08(4) .
N2 C72 1.21(4) .
