#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:58:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179087 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/49/4304932.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_4304932
loop_
_publ_author_name
'Hyui Sul Lee'
'Sven-Oliver Hauber'
'Denis Vinduš'
'Mark Niemeyer'
_publ_contact_author_address
;
Institut für Anorganische und Analytische Chemie
Johannes Gutenberg-Universität Mainz
Duesbergweg 10-14
D-55099 Mainz
Germany
;
_publ_contact_author_email       niemeyer@uni-mainz.de
_publ_contact_author_name        'Mark Niemeyer'
_publ_section_title
;
Isostructural Potassium and Thallium Salts of Sterically Crowded Triazenes:
A Structural and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4401
_journal_page_last               4412
_journal_paper_doi               10.1021/ic800029z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C88 H84 K2 N6'
_chemical_formula_weight         1303.81
_chemical_melting_point          '225-290 deg.C (dec.)'
_chemical_name_systematic
;
((1,3-bis(3,5,3'',5''-tetramethyl-1,1':3';1''-terphenyl-2'))
(triazenido-N,N'))potassium
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.567(2)
_cell_length_b                   27.567(2)
_cell_length_c                   21.709(5)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.0
_cell_volume                     16498(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8554
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5536
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0370P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                5371
_reflns_number_total             8405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800029z-file003_5.cif
_cod_data_source_block           2d_cpentane
_cod_database_code               4304932
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.33438(4) 0.83226(4) 1.07819(5) 0.0407(3) Uani 1 1 d . . .
K2 K 0.32370(4) 0.86988(3) 0.92897(5) 0.0398(3) Uani 1 1 d . . .
N1 N 0.32753(13) 0.93163(12) 1.03238(16) 0.0317(9) Uani 1 1 d . . .
N2 N 0.28024(12) 0.93351(12) 1.04035(15) 0.0288(8) Uani 1 1 d . . .
N3 N 0.25938(12) 0.89114(12) 1.02678(16) 0.0309(8) Uani 1 1 d . . .
N4 N 0.39388(12) 0.80795(12) 0.97649(16) 0.0292(8) Uani 1 1 d . . .
N5 N 0.37338(12) 0.76597(12) 0.96383(16) 0.0306(8) Uani 1 1 d . . .
N6 N 0.32618(12) 0.76655(12) 0.97463(16) 0.0298(8) Uani 1 1 d . . .
C11 C 0.34818(16) 0.97718(15) 1.05137(19) 0.0314(11) Uani 1 1 d . . .
C12 C 0.38446(16) 0.99624(16) 1.01282(19) 0.0350(11) Uani 1 1 d . . .
C13 C 0.40831(18) 1.03866(17) 1.0304(2) 0.0511(14) Uani 1 1 d . . .
H13A H 0.4331 1.0515 1.0046 0.045(2) Uiso 1 1 calc R . .
C14 C 0.39657(19) 1.06257(18) 1.0847(2) 0.0565(15) Uani 1 1 d . . .
H14A H 0.4128 1.0917 1.0956 0.045(2) Uiso 1 1 calc R . .
C15 C 0.36085(18) 1.04355(17) 1.1233(2) 0.0463(13) Uani 1 1 d . . .
H15A H 0.3524 1.0602 1.1601 0.045(2) Uiso 1 1 calc R . .
C16 C 0.33722(16) 1.00004(16) 1.1083(2) 0.0363(11) Uani 1 1 d . . .
C21 C 0.39581(16) 0.97581(16) 0.9509(2) 0.0350(11) Uani 1 1 d . . .
C22 C 0.36222(17) 0.97846(15) 0.9035(2) 0.0375(12) Uani 1 1 d . . .
H22A H 0.3302 0.9890 0.9126 0.045(2) Uiso 1 1 calc R . .
C23 C 0.37391(18) 0.96606(15) 0.8426(2) 0.0380(11) Uani 1 1 d . . .
C24 C 0.42134(18) 0.94973(16) 0.8317(2) 0.0412(12) Uani 1 1 d . . .
H24A H 0.4303 0.9412 0.7909 0.045(2) Uiso 1 1 calc R . .
C25 C 0.45525(17) 0.94562(16) 0.8775(2) 0.0393(12) Uani 1 1 d . . .
C26 C 0.44254(16) 0.95920(15) 0.9373(2) 0.0362(11) Uani 1 1 d . . .
H26A H 0.4660 0.9571 0.9693 0.045(2) Uiso 1 1 calc R . .
C31 C 0.30436(17) 0.98038(16) 1.15778(19) 0.0355(11) Uani 1 1 d . . .
C32 C 0.25352(17) 0.98245(16) 1.1547(2) 0.0370(11) Uani 1 1 d . . .
H32A H 0.2381 0.9946 1.1187 0.045(2) Uiso 1 1 calc R . .
C33 C 0.22575(18) 0.96674(17) 1.2044(2) 0.0419(12) Uani 1 1 d . . .
C34 C 0.2481(2) 0.95025(16) 1.2573(2) 0.0456(13) Uani 1 1 d . . .
H34A H 0.2287 0.9404 1.2913 0.045(2) Uiso 1 1 calc R . .
C35 C 0.29837(19) 0.94771(16) 1.2619(2) 0.0416(12) Uani 1 1 d . . .
C36 C 0.32531(18) 0.96313(15) 1.2115(2) 0.0380(12) Uani 1 1 d . . .
H36A H 0.3597 0.9618 1.2140 0.045(2) Uiso 1 1 calc R . .
C41 C 0.20760(15) 0.89550(15) 1.0310(2) 0.0336(11) Uani 1 1 d . . .
C42 C 0.17930(16) 0.92934(16) 0.9976(2) 0.0395(12) Uani 1 1 d . . .
C43 C 0.12872(18) 0.92643(19) 1.0031(3) 0.0605(16) Uani 1 1 d . . .
H43A H 0.1094 0.9498 0.9824 0.045(2) Uiso 1 1 calc R . .
C44 C 0.10592(19) 0.8915(2) 1.0370(3) 0.0723(19) Uani 1 1 d . . .
H44A H 0.0715 0.8899 1.0384 0.045(2) Uiso 1 1 calc R . .
C45 C 0.13384(16) 0.85863(18) 1.0690(3) 0.0562(15) Uani 1 1 d . . .
H45A H 0.1184 0.8347 1.0936 0.045(2) Uiso 1 1 calc R . .
C46 C 0.18460(15) 0.85974(15) 1.0660(2) 0.0356(11) Uani 1 1 d . . .
C51 C 0.19955(18) 0.96661(17) 0.9544(2) 0.0424(12) Uani 1 1 d . . .
C52 C 0.22689(17) 1.00668(16) 0.9733(2) 0.0416(12) Uani 1 1 d . . .
H52A H 0.2341 1.0106 1.0158 0.045(2) Uiso 1 1 calc R . .
C53 C 0.24367(17) 1.04072(16) 0.9314(2) 0.0446(12) Uani 1 1 d . . .
C54 C 0.23172(19) 1.03579(18) 0.8692(3) 0.0541(15) Uani 1 1 d . . .
H54A H 0.2429 1.0593 0.8405 0.045(2) Uiso 1 1 calc R . .
C55 C 0.2035(2) 0.9968(2) 0.8485(2) 0.0574(15) Uani 1 1 d . . .
C56 C 0.18827(19) 0.96257(19) 0.8917(3) 0.0517(14) Uani 1 1 d . . .
H56A H 0.1696 0.9356 0.8782 0.045(2) Uiso 1 1 calc R . .
C61 C 0.21258(15) 0.82273(16) 1.10232(19) 0.0315(10) Uani 1 1 d . . .
C62 C 0.20940(14) 0.77416(15) 1.0851(2) 0.0356(11) Uani 1 1 d . . .
H62A H 0.1919 0.7656 1.0490 0.045(2) Uiso 1 1 calc R . .
C63 C 0.23180(16) 0.73740(16) 1.1203(2) 0.0352(11) Uani 1 1 d . . .
C64 C 0.25748(16) 0.75141(17) 1.1731(2) 0.0394(12) Uani 1 1 d . . .
H64A H 0.2726 0.7271 1.1975 0.045(2) Uiso 1 1 calc R . .
C65 C 0.26162(16) 0.79973(17) 1.1912(2) 0.0381(12) Uani 1 1 d . . .
C66 C 0.23883(16) 0.83467(16) 1.1547(2) 0.0383(12) Uani 1 1 d . . .
H66A H 0.2414 0.8678 1.1662 0.045(2) Uiso 1 1 calc R . .
C71 C 0.44406(15) 0.80535(15) 0.9607(2) 0.0289(10) Uani 1 1 d . . .
C72 C 0.46028(15) 0.79052(16) 0.9030(2) 0.0350(11) Uani 1 1 d . . .
C73 C 0.51055(16) 0.79032(17) 0.8907(2) 0.0437(12) Uani 1 1 d . . .
H73A H 0.5220 0.7790 0.8520 0.045(2) Uiso 1 1 calc R . .
C74 C 0.54366(16) 0.80645(18) 0.9347(2) 0.0480(13) Uani 1 1 d . . .
H74A H 0.5774 0.8065 0.9259 0.045(2) Uiso 1 1 calc R . .
C75 C 0.52685(16) 0.82243(17) 0.9911(2) 0.0401(11) Uani 1 1 d . . .
H75A H 0.5495 0.8340 1.0207 0.045(2) Uiso 1 1 calc R . .
C76 C 0.47786(15) 0.82207(16) 1.00571(19) 0.0320(10) Uani 1 1 d . . .
C81 C 0.42699(15) 0.77919(18) 0.8496(2) 0.0379(12) Uani 1 1 d . . .
C82 C 0.40629(16) 0.73347(18) 0.8405(2) 0.0435(12) Uani 1 1 d . . .
H82A H 0.4124 0.7081 0.8691 0.045(2) Uiso 1 1 calc R . .
C83 C 0.37677(17) 0.7248(2) 0.7896(2) 0.0480(13) Uani 1 1 d . . .
C84 C 0.36993(18) 0.7605(2) 0.7467(2) 0.0519(14) Uani 1 1 d . . .
H84A H 0.3505 0.7538 0.7115 0.045(2) Uiso 1 1 calc R . .
C85 C 0.39088(17) 0.8073(2) 0.7530(2) 0.0466(13) Uani 1 1 d . . .
C86 C 0.41917(16) 0.81472(18) 0.80555(19) 0.0400(12) Uani 1 1 d . . .
H86A H 0.4337 0.8456 0.8114 0.045(2) Uiso 1 1 calc R . .
C91 C 0.46077(14) 0.83594(16) 1.0684(2) 0.0338(10) Uani 1 1 d . . .
C92 C 0.44269(15) 0.80181(17) 1.1091(2) 0.0379(11) Uani 1 1 d . . .
H92A H 0.4387 0.7693 1.0957 0.045(2) Uiso 1 1 calc R . .
C93 C 0.43011(17) 0.81402(18) 1.1697(2) 0.0428(13) Uani 1 1 d . . .
C94 C 0.43564(16) 0.86214(19) 1.1876(2) 0.0441(13) Uani 1 1 d . . .
H94A H 0.4269 0.8712 1.2283 0.045(2) Uiso 1 1 calc R . .
C95 C 0.45323(17) 0.89676(18) 1.1485(2) 0.0454(13) Uani 1 1 d . . .
C96 C 0.46609(15) 0.88380(16) 1.0888(2) 0.0385(11) Uani 1 1 d . . .
H96A H 0.4786 0.9077 1.0616 0.045(2) Uiso 1 1 calc R . .
C101 C 0.30713(15) 0.71824(14) 0.9655(2) 0.0311(10) Uani 1 1 d . . .
C102 C 0.26299(15) 0.71432(15) 0.9320(2) 0.0323(10) Uani 1 1 d . . .
C103 C 0.24129(16) 0.66857(15) 0.9243(2) 0.0402(11) Uani 1 1 d . . .
H10A H 0.2119 0.6659 0.9017 0.045(2) Uiso 1 1 calc R . .
C104 C 0.26202(18) 0.62761(17) 0.9491(2) 0.0469(13) Uani 1 1 d . . .
H10B H 0.2473 0.5968 0.9432 0.045(2) Uiso 1 1 calc R . .
C105 C 0.30536(16) 0.63165(16) 0.9833(2) 0.0424(12) Uani 1 1 d . . .
H10C H 0.3196 0.6032 1.0002 0.045(2) Uiso 1 1 calc R . .
C106 C 0.32764(15) 0.67632(15) 0.9929(2) 0.0330(11) Uani 1 1 d . . .
C111 C 0.23847(15) 0.75659(16) 0.90283(19) 0.0326(11) Uani 1 1 d . . .
C112 C 0.18896(15) 0.76386(17) 0.9112(2) 0.0410(12) Uani 1 1 d . . .
H11A H 0.1716 0.7428 0.9379 0.045(2) Uiso 1 1 calc R . .
C113 C 0.16438(17) 0.8010(2) 0.8818(2) 0.0514(14) Uani 1 1 d . . .
C114 C 0.18908(19) 0.83112(19) 0.8432(2) 0.0487(13) Uani 1 1 d . . .
H11B H 0.1724 0.8570 0.8236 0.045(2) Uiso 1 1 calc R . .
C115 C 0.23847(18) 0.82444(17) 0.8321(2) 0.0421(12) Uani 1 1 d . . .
C116 C 0.26292(17) 0.78701(16) 0.8619(2) 0.0376(11) Uani 1 1 d . . .
H11C H 0.2965 0.7822 0.8543 0.045(2) Uiso 1 1 calc R . .
C117 C 0.10990(18) 0.8076(2) 0.8927(3) 0.082(2) Uani 1 1 d . . .
H11D H 0.0958 0.8261 0.8586 0.124(4) Uiso 1 1 calc R . .
H11E H 0.1048 0.8252 0.9314 0.124(4) Uiso 1 1 calc R . .
H11F H 0.0943 0.7757 0.8952 0.124(4) Uiso 1 1 calc R . .
C118 C 0.2650(2) 0.85806(18) 0.7881(3) 0.0692(17) Uani 1 1 d . . .
H11G H 0.2521 0.8539 0.7464 0.124(4) Uiso 1 1 calc R . .
H11H H 0.2997 0.8503 0.7884 0.124(4) Uiso 1 1 calc R . .
H11I H 0.2604 0.8918 0.8012 0.124(4) Uiso 1 1 calc R . .
C121 C 0.36983(16) 0.67536(15) 1.0365(2) 0.0339(11) Uani 1 1 d . . .
C122 C 0.36082(17) 0.66250(18) 1.0984(2) 0.0468(13) Uani 1 1 d . . .
H12A H 0.3282 0.6581 1.1113 0.045(2) Uiso 1 1 calc R . .
C123 C 0.39766(19) 0.65598(19) 1.1413(3) 0.0553(14) Uani 1 1 d . . .
C124 C 0.44556(19) 0.66336(18) 1.1206(3) 0.0574(16) Uani 1 1 d . . .
H12B H 0.4716 0.6598 1.1490 0.045(2) Uiso 1 1 calc R . .
C125 C 0.45569(16) 0.67559(17) 1.0606(2) 0.0441(13) Uani 1 1 d . . .
C126 C 0.41837(15) 0.68187(15) 1.0193(2) 0.0393(12) Uani 1 1 d . . .
H12C H 0.4257 0.6909 0.9781 0.045(2) Uiso 1 1 calc R . .
C127 C 0.3854(2) 0.6410(3) 1.2071(3) 0.094(2) Uani 1 1 d . . .
H12D H 0.3617 0.6145 1.2063 0.124(4) Uiso 1 1 calc R . .
H12E H 0.3716 0.6687 1.2293 0.124(4) Uiso 1 1 calc R . .
H12F H 0.4150 0.6301 1.2281 0.124(4) Uiso 1 1 calc R . .
C128 C 0.50785(17) 0.6839(2) 1.0390(3) 0.0760(19) Uani 1 1 d . . .
H12G H 0.5304 0.6698 1.0690 0.124(4) Uiso 1 1 calc R . .
H12H H 0.5140 0.7188 1.0355 0.124(4) Uiso 1 1 calc R . .
H12I H 0.5126 0.6685 0.9988 0.124(4) Uiso 1 1 calc R . .
C231 C 0.33845(19) 0.97210(18) 0.7908(2) 0.0538(14) Uani 1 1 d . . .
H23A H 0.3375 0.9423 0.7662 0.124(4) Uiso 1 1 calc R . .
H23B H 0.3486 0.9993 0.7647 0.124(4) Uiso 1 1 calc R . .
H23C H 0.3061 0.9787 0.8076 0.124(4) Uiso 1 1 calc R . .
C251 C 0.50660(18) 0.92665(19) 0.8639(2) 0.0604(15) Uani 1 1 d . . .
H25A H 0.5151 0.9339 0.8211 0.124(4) Uiso 1 1 calc R . .
H25B H 0.5076 0.8915 0.8705 0.124(4) Uiso 1 1 calc R . .
H25C H 0.5298 0.9425 0.8915 0.124(4) Uiso 1 1 calc R . .
C331 C 0.16946(17) 0.9679(2) 1.1988(3) 0.0616(16) Uani 1 1 d . . .
H33A H 0.1552 0.9476 1.2311 0.124(4) Uiso 1 1 calc R . .
H33B H 0.1598 0.9554 1.1583 0.124(4) Uiso 1 1 calc R . .
H33C H 0.1580 1.0013 1.2033 0.124(4) Uiso 1 1 calc R . .
C351 C 0.3226(2) 0.93085(19) 1.3209(2) 0.0592(15) Uani 1 1 d . . .
H35A H 0.3553 0.9190 1.3116 0.124(4) Uiso 1 1 calc R . .
H35B H 0.3035 0.9046 1.3393 0.124(4) Uiso 1 1 calc R . .
H35C H 0.3246 0.9580 1.3499 0.124(4) Uiso 1 1 calc R . .
C531 C 0.2738(2) 1.08277(17) 0.9538(2) 0.0618(16) Uani 1 1 d . . .
H53A H 0.2546 1.1027 0.9820 0.124(4) Uiso 1 1 calc R . .
H53B H 0.2840 1.1025 0.9185 0.124(4) Uiso 1 1 calc R . .
H53C H 0.3025 1.0705 0.9753 0.124(4) Uiso 1 1 calc R . .
C551 C 0.1908(2) 0.9922(2) 0.7802(3) 0.083(2) Uani 1 1 d . . .
H55A H 0.2177 1.0044 0.7552 0.124(4) Uiso 1 1 calc R . .
H55B H 0.1615 1.0111 0.7715 0.124(4) Uiso 1 1 calc R . .
H55C H 0.1849 0.9580 0.7702 0.124(4) Uiso 1 1 calc R . .
C631 C 0.22567(17) 0.68474(15) 1.1019(2) 0.0449(13) Uani 1 1 d . . .
H63A H 0.1915 0.6784 1.0925 0.124(4) Uiso 1 1 calc R . .
H63B H 0.2361 0.6638 1.1358 0.124(4) Uiso 1 1 calc R . .
H63C H 0.2454 0.6780 1.0653 0.124(4) Uiso 1 1 calc R . .
C651 C 0.28805(19) 0.81352(19) 1.2503(2) 0.0565(15) Uani 1 1 d . . .
H65A H 0.3131 0.8376 1.2410 0.124(4) Uiso 1 1 calc R . .
H65B H 0.3032 0.7846 1.2681 0.124(4) Uiso 1 1 calc R . .
H65C H 0.2649 0.8272 1.2797 0.124(4) Uiso 1 1 calc R . .
C831 C 0.3542(2) 0.6751(2) 0.7812(3) 0.079(2) Uani 1 1 d . . .
H83A H 0.3433 0.6714 0.7385 0.124(4) Uiso 1 1 calc R . .
H83B H 0.3264 0.6717 0.8090 0.124(4) Uiso 1 1 calc R . .
H83C H 0.3783 0.6501 0.7906 0.124(4) Uiso 1 1 calc R . .
C851 C 0.3850(2) 0.8463(2) 0.7054(2) 0.0691(18) Uani 1 1 d . . .
H85A H 0.3886 0.8781 0.7250 0.124(4) Uiso 1 1 calc R . .
H85B H 0.3527 0.8438 0.6868 0.124(4) Uiso 1 1 calc R . .
H85C H 0.4098 0.8424 0.6735 0.124(4) Uiso 1 1 calc R . .
C931 C 0.4138(2) 0.7753(2) 1.2143(2) 0.0654(17) Uani 1 1 d . . .
H93A H 0.3976 0.7905 1.2495 0.124(4) Uiso 1 1 calc R . .
H93B H 0.4420 0.7569 1.2288 0.124(4) Uiso 1 1 calc R . .
H93C H 0.3911 0.7532 1.1936 0.124(4) Uiso 1 1 calc R . .
C951 C 0.4620(2) 0.94881(18) 1.1703(3) 0.0650(16) Uani 1 1 d . . .
H95A H 0.4450 0.9714 1.1430 0.124(4) Uiso 1 1 calc R . .
H95B H 0.4968 0.9558 1.1696 0.124(4) Uiso 1 1 calc R . .
H95C H 0.4497 0.9526 1.2124 0.124(4) 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'
N N 0.0061 0.0033 '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'
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
N4 K1 N3 104.44(10) . . ?
N4 K1 N6 44.91(9) . . ?
N3 K1 N6 89.75(10) . . ?
N4 K1 N1 89.66(10) . . ?
N3 K1 N1 44.52(10) . . ?
N6 K1 N1 108.51(10) . . ?
N4 K1 C66 155.64(11) . . ?
N3 K1 C66 65.42(11) . . ?
N6 K1 C66 111.18(11) . . ?
N1 K1 C66 96.13(11) . . ?
N4 K1 C92 63.73(11) . . ?
N3 K1 C92 156.11(11) . . ?
N6 K1 C92 94.15(11) . . ?
N1 K1 C92 112.40(11) . . ?
C66 K1 C92 133.50(12) . . ?
N4 K1 N5 23.60(8) . . ?
N3 K1 N5 105.04(10) . . ?
N6 K1 N5 23.84(8) . . ?
N1 K1 N5 106.71(10) . . ?
C66 K1 N5 134.11(11) . . ?
C92 K1 N5 72.73(11) . . ?
N4 K1 N2 105.70(9) . . ?
N3 K1 N2 23.97(8) . . ?
N6 K1 N2 107.66(10) . . ?
N1 K1 N2 23.69(8) . . ?
C66 K1 N2 74.32(10) . . ?
C92 K1 N2 135.10(11) . . ?
N5 K1 N2 115.92(9) . . ?
N4 K1 C65 150.39(11) . . ?
N3 K1 C65 90.28(11) . . ?
N6 K1 C65 111.12(11) . . ?
N1 K1 C65 118.01(11) . . ?
C66 K1 C65 24.97(11) . . ?
C92 K1 C65 110.07(12) . . ?
N5 K1 C65 127.92(11) . . ?
N2 K1 C65 98.14(11) . . ?
N4 K1 C93 88.30(11) . . ?
N3 K1 C93 152.84(12) . . ?
N6 K1 C93 115.41(11) . . ?
N1 K1 C93 113.24(12) . . ?
C66 K1 C93 110.74(12) . . ?
C92 K1 C93 24.65(11) . . ?
N5 K1 C93 96.18(11) . . ?
N2 K1 C93 129.66(11) . . ?
C65 K1 C93 89.85(12) . . ?
N4 K1 C61 132.26(10) . . ?
N3 K1 C61 52.46(10) . . ?
N6 K1 C61 89.67(10) . . ?
N1 K1 C61 93.49(10) . . ?
C66 K1 C61 24.02(10) . . ?
C92 K1 C61 150.91(11) . . ?
N5 K1 C61 113.47(10) . . ?
N2 K1 C61 69.80(9) . . ?
C65 K1 C61 42.65(11) . . ?
C93 K1 C61 132.47(12) . . ?
N4 K1 K2 51.82(7) . . ?
N3 K1 K2 52.71(7) . . ?
N6 K1 K2 56.41(7) . . ?
N1 K1 K2 52.15(7) . . ?
C66 K1 K2 115.25(9) . . ?
C92 K1 K2 111.25(9) . . ?
N5 K1 K2 58.46(6) . . ?
N2 K1 K2 57.52(6) . . ?
C65 K1 K2 137.48(9) . . ?
C93 K1 K2 132.68(9) . . ?
C61 K1 K2 94.84(8) . . ?
N4 K2 N1 92.83(10) . . ?
N4 K2 N3 106.57(10) . . ?
N1 K2 N3 45.61(10) . . ?
N4 K2 N6 44.13(9) . . ?
N1 K2 N6 107.92(10) . . ?
N3 K2 N6 87.89(10) . . ?
N4 K2 C116 95.47(11) . . ?
N1 K2 C116 144.75(11) . . ?
N3 K2 C116 99.32(11) . . ?
N6 K2 C116 58.99(11) . . ?
N4 K2 N2 108.37(10) . . ?
N1 K2 N2 24.03(9) . . ?
N3 K2 N2 24.43(8) . . ?
N6 K2 N2 106.03(9) . . ?
C116 K2 N2 122.58(11) . . ?
N4 K2 C22 113.87(11) . . ?
N1 K2 C22 64.12(11) . . ?
N3 K2 C22 98.21(11) . . ?
N6 K2 C22 157.75(11) . . ?
C116 K2 C22 139.54(12) . . ?
N2 K2 C22 75.25(10) . . ?
N4 K2 N5 23.46(9) . . ?
N1 K2 N5 109.25(10) . . ?
N3 K2 N5 105.72(10) . . ?
N6 K2 N5 23.89(8) . . ?
C116 K2 N5 72.38(11) . . ?
N2 K2 N5 117.41(9) . . ?
C22 K2 N5 135.75(11) . . ?
N4 K2 C115 119.04(11) . . ?
N1 K2 C115 137.94(12) . . ?
N3 K2 C115 96.19(12) . . ?
N6 K2 C115 82.58(11) . . ?
C116 K2 C115 24.17(11) . . ?
N2 K2 C115 114.15(11) . . ?
C22 K2 C115 117.68(12) . . ?
N5 K2 C115 96.34(10) . . ?
N4 K2 K1 53.21(7) . . ?
N1 K2 K1 54.88(7) . . ?
N3 K2 K1 53.45(7) . . ?
N6 K2 K1 53.09(7) . . ?
C116 K2 K1 105.14(9) . . ?
N2 K2 K1 58.99(6) . . ?
C22 K2 K1 114.60(9) . . ?
N5 K2 K1 58.48(6) . . ?
C115 K2 K1 122.40(9) . . ?
N4 K2 C23 112.68(11) . . ?
N1 K2 C23 87.40(10) . . ?
N3 K2 C23 119.27(10) . . ?
N6 K2 C23 151.03(11) . . ?
C116 K2 C23 120.15(11) . . ?
N2 K2 C23 97.79(10) . . ?
C22 K2 C23 23.41(10) . . ?
N5 K2 C23 128.16(11) . . ?
C115 K2 C23 102.68(11) . . ?
K1 K2 C23 134.29(8) . . ?
N2 N1 C11 108.7(3) . . ?
N2 N1 K2 95.2(2) . . ?
C11 N1 K2 140.3(3) . . ?
N2 N1 K1 93.2(2) . . ?
C11 N1 K1 134.1(3) . . ?
K2 N1 K1 72.97(8) . . ?
N1 N2 N3 111.3(3) . . ?
N1 N2 K2 60.7(2) . . ?
N3 N2 K2 61.16(19) . . ?
N1 N2 K1 63.1(2) . . ?
N3 N2 K1 60.34(19) . . ?
K2 N2 K1 63.49(7) . . ?
N2 N3 C41 109.9(3) . . ?
N2 N3 K2 94.4(2) . . ?
C41 N3 K2 133.6(3) . . ?
N2 N3 K1 95.7(2) . . ?
C41 N3 K1 137.9(3) . . ?
K2 N3 K1 73.84(8) . . ?
N5 N4 C71 108.7(3) . . ?
N5 N4 K2 99.4(2) . . ?
C71 N4 K2 128.0(3) . . ?
N5 N4 K1 97.0(2) . . ?
C71 N4 K1 139.6(3) . . ?
K2 N4 K1 74.97(9) . . ?
N4 N5 N6 112.0(3) . . ?
N4 N5 K2 57.12(19) . . ?
N6 N5 K2 67.5(2) . . ?
N4 N5 K1 59.4(2) . . ?
N6 N5 K1 62.2(2) . . ?
K2 N5 K1 63.05(7) . . ?
N5 N6 C101 108.8(3) . . ?
N5 N6 K1 93.9(2) . . ?
C101 N6 K1 135.4(3) . . ?
N5 N6 K2 88.6(2) . . ?
C101 N6 K2 144.8(3) . . ?
K1 N6 K2 70.50(8) . . ?
C12 C11 C16 120.2(4) . . ?
C12 C11 N1 115.9(4) . . ?
C16 C11 N1 123.5(4) . . ?
C13 C12 C11 119.1(4) . . ?
C13 C12 C21 117.7(4) . . ?
C11 C12 C21 123.0(4) . . ?
C14 C13 C12 121.3(4) . . ?
C13 C14 C15 119.7(4) . . ?
C14 C15 C16 120.6(4) . . ?
C15 C16 C11 118.9(4) . . ?
C15 C16 C31 114.9(4) . . ?
C11 C16 C31 126.1(4) . . ?
C22 C21 C26 118.4(4) . . ?
C22 C21 C12 120.6(4) . . ?
C26 C21 C12 120.5(4) . . ?
C21 C22 C23 122.2(4) . . ?
C21 C22 K2 92.5(3) . . ?
C23 C22 K2 90.6(3) . . ?
C22 C23 C24 116.8(4) . . ?
C22 C23 C231 122.0(4) . . ?
C24 C23 C231 121.1(4) . . ?
C22 C23 K2 65.9(2) . . ?
C24 C23 K2 102.4(3) . . ?
C231 C23 K2 103.1(3) . . ?
C25 C24 C23 122.7(4) . . ?
C24 C25 C26 118.8(4) . . ?
C24 C25 C251 121.1(4) . . ?
C26 C25 C251 120.1(4) . . ?
C25 C26 C21 121.0(4) . . ?
C36 C31 C32 118.0(4) . . ?
C36 C31 C16 118.3(4) . . ?
C32 C31 C16 123.5(4) . . ?
C33 C32 C31 120.0(4) . . ?
C34 C33 C32 120.2(5) . . ?
C34 C33 C331 121.0(5) . . ?
C32 C33 C331 118.8(5) . . ?
C33 C34 C35 121.3(5) . . ?
C36 C35 C34 117.5(5) . . ?
C36 C35 C351 121.6(5) . . ?
C34 C35 C351 120.9(4) . . ?
C31 C36 C35 123.0(5) . . ?
C46 C41 C42 119.6(4) . . ?
C46 C41 N3 115.3(4) . . ?
C42 C41 N3 124.8(4) . . ?
C43 C42 C41 117.8(4) . . ?
C43 C42 C51 117.6(4) . . ?
C41 C42 C51 124.5(4) . . ?
C44 C43 C42 123.0(5) . . ?
C43 C44 C45 118.6(5) . . ?
C44 C45 C46 121.3(5) . . ?
C41 C46 C45 119.6(4) . . ?
C41 C46 C61 122.1(4) . . ?
C45 C46 C61 118.2(4) . . ?
C52 C51 C56 117.8(5) . . ?
C52 C51 C42 124.0(4) . . ?
C56 C51 C42 118.1(5) . . ?
C53 C52 C51 121.6(5) . . ?
C52 C53 C54 119.3(5) . . ?
C52 C53 C531 119.7(5) . . ?
C54 C53 C531 121.1(5) . . ?
C53 C54 C55 121.1(5) . . ?
C56 C55 C54 118.1(5) . . ?
C56 C55 C551 121.7(6) . . ?
C54 C55 C551 120.2(5) . . ?
C55 C56 C51 122.2(5) . . ?
C66 C61 C62 118.7(4) . . ?
C66 C61 C46 122.5(4) . . ?
C62 C61 C46 118.7(4) . . ?
C66 C61 K1 66.0(2) . . ?
C62 C61 K1 95.4(3) . . ?
C46 C61 K1 111.9(2) . . ?
C61 C62 C63 121.1(4) . . ?
C64 C63 C62 117.8(4) . . ?
C64 C63 C631 122.5(4) . . ?
C62 C63 C631 119.7(4) . . ?
C65 C64 C63 122.3(4) . . ?
C64 C65 C66 117.6(4) . . ?
C64 C65 C651 121.0(4) . . ?
C66 C65 C651 121.4(4) . . ?
C64 C65 K1 95.8(3) . . ?
C66 C65 K1 70.4(2) . . ?
C651 C65 K1 105.5(3) . . ?
C61 C66 C65 122.4(4) . . ?
C61 C66 K1 89.9(3) . . ?
C65 C66 K1 84.7(3) . . ?
C72 C71 N4 122.9(4) . . ?
C72 C71 C76 120.1(4) . . ?
N4 C71 C76 116.8(4) . . ?
C71 C72 C73 119.1(4) . . ?
C71 C72 C81 123.8(4) . . ?
C73 C72 C81 116.8(4) . . ?
C74 C73 C72 120.8(4) . . ?
C75 C74 C73 119.3(4) . . ?
C74 C75 C76 121.8(4) . . ?
C75 C76 C71 118.8(4) . . ?
C75 C76 C91 121.0(4) . . ?
C71 C76 C91 120.2(4) . . ?
C86 C81 C82 118.4(4) . . ?
C86 C81 C72 118.5(4) . . ?
C82 C81 C72 122.9(4) . . ?
C83 C82 C81 120.3(5) . . ?
C84 C83 C82 119.9(5) . . ?
C84 C83 C831 120.7(5) . . ?
C82 C83 C831 119.3(5) . . ?
C83 C84 C85 122.1(5) . . ?
C86 C85 C84 116.1(5) . . ?
C86 C85 C851 121.2(5) . . ?
C84 C85 C851 122.7(5) . . ?
C81 C86 C85 123.1(5) . . ?
C92 C91 C96 118.4(4) . . ?
C92 C91 C76 121.6(4) . . ?
C96 C91 C76 119.9(4) . . ?
C92 C91 K1 65.3(2) . . ?
C96 C91 K1 96.5(3) . . ?
C76 C91 K1 111.3(2) . . ?
C91 C92 C93 121.7(4) . . ?
C91 C92 K1 91.4(3) . . ?
C93 C92 K1 84.4(3) . . ?
C94 C93 C92 117.7(5) . . ?
C94 C93 C931 121.9(5) . . ?
C92 C93 C931 120.4(5) . . ?
C94 C93 K1 96.3(3) . . ?
C92 C93 K1 71.0(3) . . ?
C931 C93 K1 104.6(3) . . ?
C95 C94 C93 122.1(5) . . ?
C94 C95 C96 119.4(5) . . ?
C94 C95 C951 121.2(5) . . ?
C96 C95 C951 119.3(5) . . ?
C95 C96 C91 120.7(5) . . ?
C106 C101 C102 119.6(4) . . ?
C106 C101 N6 123.3(4) . . ?
C102 C101 N6 116.8(4) . . ?
C103 C102 C101 119.5(4) . . ?
C103 C102 C111 117.3(4) . . ?
C101 C102 C111 123.1(4) . . ?
C104 C103 C102 120.9(4) . . ?
C103 C104 C105 119.5(4) . . ?
C106 C105 C104 121.5(4) . . ?
C105 C106 C101 118.8(4) . . ?
C105 C106 C121 114.9(4) . . ?
C101 C106 C121 126.1(4) . . ?
C112 C111 C116 118.1(4) . . ?
C112 C111 C102 120.2(4) . . ?
C116 C111 C102 121.5(4) . . ?
C113 C112 C111 121.8(5) . . ?
C114 C113 C112 119.3(5) . . ?
C114 C113 C117 120.8(5) . . ?
C112 C113 C117 119.8(5) . . ?
C113 C114 C115 120.9(5) . . ?
C116 C115 C114 119.3(5) . . ?
C116 C115 C118 120.7(5) . . ?
C114 C115 C118 119.9(5) . . ?
C116 C115 K2 69.5(3) . . ?
C114 C115 K2 121.3(3) . . ?
C118 C115 K2 80.2(3) . . ?
C115 C116 C111 120.5(4) . . ?
C115 C116 K2 86.3(3) . . ?
C111 C116 K2 113.2(3) . . ?
C126 C121 C122 117.0(4) . . ?
C126 C121 C106 124.8(4) . . ?
C122 C121 C106 118.0(4) . . ?
C123 C122 C121 122.8(5) . . ?
C122 C123 C124 116.9(5) . . ?
C122 C123 C127 120.1(5) . . ?
C124 C123 C127 123.0(5) . . ?
C125 C124 C123 121.9(5) . . ?
C124 C125 C126 119.8(5) . . ?
C124 C125 C128 121.2(5) . . ?
C126 C125 C128 119.0(5) . . ?
C125 C126 C121 121.7(5) . . ?
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
K1 N4 2.831(4) . ?
K1 N3 2.856(3) . ?
K1 N6 2.896(4) . ?
K1 N1 2.920(3) . ?
K1 C66 3.115(4) . ?
K1 C92 3.174(4) . ?
K1 N5 3.265(4) . ?
K1 N2 3.270(3) . ?
K1 C65 3.293(4) . ?
K1 C93 3.341(5) . ?
K1 C61 3.408(4) . ?
K1 K2 3.4139(15) . ?
K2 N4 2.779(3) . ?
K2 N1 2.819(4) . ?
K2 N3 2.828(3) . ?
K2 N6 3.017(3) . ?
K2 C116 3.185(4) . ?
K2 N2 3.218(4) . ?
K2 C22 3.224(4) . ?
K2 N5 3.264(4) . ?
K2 C115 3.394(5) . ?
K2 C23 3.530(4) . ?
N1 N2 1.316(4) . ?
N1 C11 1.439(5) . ?
N2 N3 1.335(4) . ?
N3 C41 1.435(5) . ?
N4 N5 1.317(4) . ?
N4 C71 1.427(5) . ?
N5 N6 1.322(4) . ?
N6 C101 1.445(5) . ?
C11 C12 1.406(6) . ?
C11 C16 1.419(6) . ?
C12 C13 1.395(6) . ?
C12 C21 1.490(6) . ?
C13 C14 1.390(6) . ?
C14 C15 1.394(6) . ?
C15 C16 1.404(6) . ?
C16 C31 1.506(6) . ?
C21 C22 1.386(6) . ?
C21 C26 1.399(6) . ?
C22 C23 1.403(6) . ?
C23 C24 1.403(6) . ?
C23 C231 1.500(6) . ?
C24 C25 1.370(6) . ?
C25 C26 1.396(6) . ?
C25 C251 1.538(6) . ?
C31 C36 1.386(6) . ?
C31 C32 1.404(6) . ?
C32 C33 1.391(6) . ?
C33 C34 1.382(6) . ?
C33 C331 1.557(6) . ?
C34 C35 1.392(7) . ?
C35 C36 1.389(6) . ?
C35 C351 1.517(6) . ?
C41 C46 1.396(6) . ?
C41 C42 1.416(6) . ?
C42 C43 1.402(7) . ?
C42 C51 1.499(6) . ?
C43 C44 1.364(7) . ?
C44 C45 1.378(7) . ?
C45 C46 1.401(6) . ?
C46 C61 1.502(6) . ?
C51 C52 1.398(6) . ?
C51 C56 1.401(7) . ?
C52 C53 1.385(6) . ?
C53 C54 1.397(7) . ?
C53 C531 1.507(7) . ?
C54 C55 1.401(7) . ?
C55 C56 1.395(7) . ?
C55 C551 1.529(7) . ?
C61 C66 1.388(6) . ?
C61 C62 1.393(6) . ?
C62 C63 1.412(6) . ?
C63 C64 1.401(6) . ?
C63 C631 1.516(6) . ?
C64 C65 1.393(6) . ?
C65 C66 1.396(6) . ?
C65 C651 1.523(6) . ?
C71 C72 1.390(6) . ?
C71 C76 1.427(6) . ?
C72 C73 1.411(6) . ?
C72 C81 1.512(6) . ?
C73 C74 1.393(6) . ?
C74 C75 1.382(6) . ?
C75 C76 1.387(6) . ?
C76 C91 1.489(6) . ?
C81 C86 1.385(6) . ?
C81 C82 1.398(6) . ?
C82 C83 1.392(6) . ?
C83 C84 1.368(7) . ?
C83 C831 1.517(7) . ?
C84 C85 1.419(7) . ?
C85 C86 1.397(6) . ?
C85 C851 1.500(7) . ?
C91 C92 1.385(6) . ?
C91 C96 1.400(6) . ?
C92 C93 1.400(6) . ?
C93 C94 1.391(6) . ?
C93 C931 1.512(7) . ?
C94 C95 1.366(6) . ?
C95 C96 1.389(6) . ?
C95 C951 1.530(7) . ?
C101 C106 1.418(6) . ?
C101 C102 1.421(6) . ?
C102 C103 1.406(5) . ?
C102 C111 1.488(6) . ?
C103 C104 1.375(6) . ?
C104 C105 1.411(6) . ?
C105 C106 1.392(6) . ?
C106 C121 1.500(6) . ?
C111 C112 1.392(6) . ?
C111 C116 1.395(6) . ?
C112 C113 1.383(6) . ?
C113 C114 1.363(7) . ?
C113 C117 1.531(7) . ?
C114 C115 1.395(6) . ?
C115 C116 1.393(6) . ?
C115 C118 1.518(7) . ?
C121 C126 1.401(6) . ?
C121 C122 1.412(6) . ?
C122 C123 1.390(7) . ?
C123 C124 1.410(7) . ?
C123 C127 1.525(7) . ?
C124 C125 1.375(7) . ?
C125 C126 1.375(6) . ?
C125 C128 1.530(6) . ?
