#------------------------------------------------------------------------------
#$Date: 2019-11-16 06:29:43 +0200 (Sat, 16 Nov 2019) $
#$Revision: 227934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/90/7059048.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_7059048
loop_
_publ_author_name
'Konarev, Dmitri V.'
'Faraonov, Maxim A.'
'Kuz`min, Alexey V.'
'Osipov, Nikita G.'
'Khasanov, Salavat S.'
'Otsuka, Akihiro'
'Yamochi, Hideki'
'Kitagawa, Hiroshi'
'Lyubovskaya, Rimma N.'
_publ_section_title
;
 Molecular structure, optical and magnetic properties of free-base
 tetrapyrazinoporphyrazine in various reduction states
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C9NJ04775A
_journal_year                    2019
_chemical_formula_moiety         'C6 H4 Cl2, 2(C18 H36 K N2 O6), 2(C12 H5 N8)'
_chemical_formula_sum            'C66 H86 Cl2 K2 N20 O12'
_chemical_formula_weight         1500.64
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-08 deposited with the CCDC.	2019-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                102.290(4)
_cell_angle_beta                 99.291(3)
_cell_angle_gamma                95.730(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8535(3)
_cell_length_b                   15.7516(7)
_cell_length_c                   24.2437(11)
_cell_measurement_reflns_used    6167
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      25.6610
_cell_measurement_theta_min      1.7600
_cell_volume                     3593.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  40.00   1.00   96.00    --   11.89 -99.00-120.00   39
  2  ω   -102.00 -66.00   1.00   96.00    --  -12.20-178.00   0.00   36
  3  ω      9.00  61.00   1.00   96.00    --  -12.20  37.00  90.00   52
  4  ω     -3.00  36.00   1.00   96.00    --  -12.20-124.00 154.00   39
  5  ω    -13.00  28.00   1.00   96.00    --  -12.20 -99.00-150.00   41
  6  ω    -88.00  23.00   1.00   96.00    --  -12.20 -19.00 -60.00  111
  7  ω    -38.00  -9.00   1.00   96.00    --  -12.20  37.00   0.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0132411000
_diffrn_orient_matrix_UB_12      0.0007385000
_diffrn_orient_matrix_UB_13      -0.0295218000
_diffrn_orient_matrix_UB_21      0.0187627000
_diffrn_orient_matrix_UB_22      -0.0427353000
_diffrn_orient_matrix_UB_23      -0.0072258000
_diffrn_orient_matrix_UB_31      -0.0699867000
_diffrn_orient_matrix_UB_32      -0.0184138000
_diffrn_orient_matrix_UB_33      -0.0023812000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.1320
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34558
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.667
_diffrn_reflns_theta_min         1.751
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       needle
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.687
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         16824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0677
_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)+(0.0177P)²+5.6375P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8843
_reflns_number_total             16824
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj04775a2.cif
_cod_data_source_block           exp_1312_int1
_cod_database_code               7059048
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C68H66N18Cl2K1V2
_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 98.95
_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 N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P), C109(H10Q,H10R),
 C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H), C114(H11I,
 H11J), C115(H11K,H11L), C116(H11M,H11N), C117(H11O,H11P), C118(H11Q,H11R),
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C207(H20M,H20N), C208(H20O,H20P), C209(H20Q,H20R),
 C210(H21A,H21B), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J), C215(H21K,H21L), C216(H21M,H21N), C217(H21O,H21P), C218(H21Q,H21R)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C54(H54), C55(H55), C56(H56), C304(H304), C305(H305), C310(H310),
 C311(H311), N301(H301), C404(H404), C405(H405), C410(H410), C411(H411),
 N401(H401)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.840
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
C51 C 0.7957(4) 0.1209(3) 0.76946(17) 0.0339(10) Uani 1 1 d .
C52 C 0.9401(4) 0.1351(3) 0.78052(16) 0.0307(9) Uani 1 1 d .
C53 C 1.0107(4) 0.2192(3) 0.80284(16) 0.0357(11) Uani 1 1 d .
H53 H 1.107291 0.228467 0.810743 0.043 Uiso 1 1 calc R
C54 C 0.9370(5) 0.2890(3) 0.81328(18) 0.0411(11) Uani 1 1 d .
H54 H 0.984159 0.345639 0.827484 0.049 Uiso 1 1 calc R
C55 C 0.7933(5) 0.2753(3) 0.80272(19) 0.0450(11) Uani 1 1 d .
H55 H 0.744143 0.322560 0.810204 0.054 Uiso 1 1 calc R
C56 C 0.7228(5) 0.1915(3) 0.78110(19) 0.0454(12) Uani 1 1 d .
H56 H 0.626296 0.182292 0.774329 0.055 Uiso 1 1 calc R
Cl51 Cl 0.70480(12) 0.01671(8) 0.74152(6) 0.0563(3) Uani 1 1 d .
Cl52 Cl 1.03400(11) 0.04858(7) 0.76552(5) 0.0435(3) Uani 1 1 d .
C101 C 0.5061(4) 0.2679(3) 0.21261(18) 0.0439(12) Uani 1 1 d .
H10A H 0.463431 0.219247 0.225484 0.053 Uiso 1 1 calc R
H10B H 0.583169 0.298697 0.242705 0.053 Uiso 1 1 calc R
C102 C 0.5611(4) 0.2323(3) 0.15913(17) 0.0417(11) Uani 1 1 d .
H10C H 0.598278 0.280323 0.144242 0.050 Uiso 1 1 calc R
H10D H 0.635348 0.198505 0.168093 0.050 Uiso 1 1 calc R
C103 C 0.5033(4) 0.1390(3) 0.06748(16) 0.0282(9) Uani 1 1 d .
H10E H 0.571126 0.101618 0.077613 0.034 Uiso 1 1 calc R
H10F H 0.548847 0.184513 0.052654 0.034 Uiso 1 1 calc R
C104 C 0.3864(4) 0.0862(2) 0.02259(16) 0.0253(8) Uani 1 1 d .
H10G H 0.422601 0.054236 -0.009391 0.030 Uiso 1 1 calc R
H10H H 0.336211 0.043838 0.038453 0.030 Uiso 1 1 calc R
C105 C 0.1968(4) 0.0951(3) -0.04665(15) 0.0277(9) Uani 1 1 d .
H10I H 0.144481 0.046008 -0.037636 0.033 Uiso 1 1 calc R
H10J H 0.245169 0.072184 -0.077200 0.033 Uiso 1 1 calc R
C106 C 0.0993(4) 0.1547(3) -0.06635(16) 0.0321(10) Uani 1 1 d .
H10K H 0.152618 0.203306 -0.075538 0.039 Uiso 1 1 calc R
H10L H 0.036469 0.122638 -0.101249 0.039 Uiso 1 1 calc R
C107 C 0.4748(4) 0.4147(3) 0.2037(2) 0.0469(13) Uani 1 1 d .
H10M H 0.548379 0.406518 0.181690 0.056 Uiso 1 1 calc R
H10N H 0.517765 0.444343 0.242856 0.056 Uiso 1 1 calc R
C108 C 0.3823(5) 0.4729(3) 0.1793(2) 0.0450(12) Uani 1 1 d .
H10O H 0.307388 0.481216 0.200521 0.054 Uiso 1 1 calc R
H10P H 0.435039 0.529959 0.183091 0.054 Uiso 1 1 calc R
C109 C 0.2513(5) 0.4941(3) 0.0948(2) 0.0452(12) Uani 1 1 d .
H10Q H 0.310639 0.549217 0.099870 0.054 Uiso 1 1 calc R
H10R H 0.172371 0.505977 0.113109 0.054 Uiso 1 1 calc R
C110 C 0.2028(5) 0.4540(3) 0.03285(19) 0.0422(12) Uani 1 1 d .
H11A H 0.162964 0.496527 0.013859 0.051 Uiso 1 1 calc R
H11B H 0.280705 0.436256 0.015506 0.051 Uiso 1 1 calc R
C111 C 0.0434(4) 0.3442(3) -0.03351(17) 0.0367(10) Uani 1 1 d .
H11C H 0.116861 0.331569 -0.054966 0.044 Uiso 1 1 calc R
H11D H -0.006922 0.386465 -0.048958 0.044 Uiso 1 1 calc R
C112 C -0.0533(4) 0.2616(3) -0.03954(18) 0.0349(10) Uani 1 1 d .
H11E H -0.122280 0.274485 -0.015733 0.042 Uiso 1 1 calc R
H11F H -0.101594 0.242051 -0.079146 0.042 Uiso 1 1 calc R
C113 C 0.3184(4) 0.3359(3) 0.24860(17) 0.0328(10) Uani 1 1 d .
H11G H 0.263624 0.383108 0.245635 0.039 Uiso 1 1 calc R
H11H H 0.379093 0.351821 0.286008 0.039 Uiso 1 1 calc R
C114 C 0.2220(4) 0.2533(3) 0.24487(16) 0.0311(9) Uani 1 1 d .
H11I H 0.275762 0.206899 0.251428 0.037 Uiso 1 1 calc R
H11J H 0.165406 0.263854 0.274214 0.037 Uiso 1 1 calc R
C115 C 0.0497(4) 0.1456(2) 0.18258(16) 0.0279(9) Uani 1 1 d .
H11K H 0.018517 0.142665 0.218177 0.033 Uiso 1 1 calc R
H11L H 0.102511 0.097526 0.172944 0.033 Uiso 1 1 calc R
C116 C -0.0728(4) 0.1377(2) 0.13560(16) 0.0285(9) Uani 1 1 d .
H11M H -0.136535 0.085378 0.133275 0.034 Uiso 1 1 calc R
H11N H -0.121459 0.188125 0.143860 0.034 Uiso 1 1 calc R
C117 C -0.1378(3) 0.1402(2) 0.03801(16) 0.0256(9) Uani 1 1 d .
H11O H -0.162878 0.198957 0.045798 0.031 Uiso 1 1 calc R
H11P H -0.218932 0.098931 0.036714 0.031 Uiso 1 1 calc R
C118 C -0.0891(4) 0.1206(2) -0.01857(16) 0.0290(9) Uani 1 1 d .
H11Q H -0.051279 0.065586 -0.023023 0.035 Uiso 1 1 calc R
H11R H -0.168081 0.113778 -0.049552 0.035 Uiso 1 1 calc R
K101 K 0.20761(8) 0.25801(5) 0.08892(3) 0.02309(19) Uani 1 1 d .
N101 N 0.4042(3) 0.3276(2) 0.20391(14) 0.0315(8) Uani 1 1 d .
N102 N 0.0169(3) 0.1900(2) -0.02322(13) 0.0266(7) Uani 1 1 d .
O101 O 0.4515(2) 0.17795(16) 0.11719(10) 0.0275(6) Uani 1 1 d .
O102 O 0.2950(2) 0.14206(16) 0.00298(10) 0.0247(6) Uani 1 1 d .
O103 O 0.3265(3) 0.43533(18) 0.12066(12) 0.0386(7) Uani 1 1 d .
O104 O 0.1017(3) 0.37984(17) 0.02566(12) 0.0354(7) Uani 1 1 d .
O105 O 0.1353(2) 0.22742(16) 0.18967(10) 0.0244(6) Uani 1 1 d .
O106 O -0.0273(2) 0.13273(16) 0.08223(10) 0.0241(6) Uani 1 1 d .
C201 C 0.1057(4) 0.3353(3) 0.66986(18) 0.0356(10) Uani 1 1 d .
H20A H 0.088444 0.345980 0.708850 0.043 Uiso 1 1 calc R
H20B H 0.020389 0.339240 0.644838 0.043 Uiso 1 1 calc R
C202 C 0.2159(4) 0.4063(3) 0.66642(18) 0.0384(11) Uani 1 1 d .
H20C H 0.186702 0.463382 0.678298 0.046 Uiso 1 1 calc R
H20D H 0.301696 0.404452 0.691865 0.046 Uiso 1 1 calc R
C203 C 0.3221(4) 0.4659(2) 0.59968(18) 0.0351(10) Uani 1 1 d .
H20E H 0.418522 0.466028 0.616363 0.042 Uiso 1 1 calc R
H20F H 0.293176 0.520576 0.617538 0.042 Uiso 1 1 calc R
C204 C 0.3062(4) 0.4569(3) 0.53657(18) 0.0345(10) Uani 1 1 d .
H20G H 0.208587 0.450882 0.519625 0.041 Uiso 1 1 calc R
H20H H 0.353265 0.509000 0.528890 0.041 Uiso 1 1 calc R
C205 C 0.3475(4) 0.3701(3) 0.45054(17) 0.0338(10) Uani 1 1 d .
H20I H 0.395368 0.420928 0.441600 0.041 Uiso 1 1 calc R
H20J H 0.249798 0.364274 0.433726 0.041 Uiso 1 1 calc R
C206 C 0.4071(4) 0.2888(2) 0.42613(17) 0.0314(9) Uani 1 1 d .
H20K H 0.415337 0.288104 0.386717 0.038 Uiso 1 1 calc R
H20L H 0.499637 0.291217 0.447893 0.038 Uiso 1 1 calc R
C207 C 0.2523(4) 0.2309(3) 0.69781(16) 0.0300(9) Uani 1 1 d .
H20M H 0.216296 0.228396 0.732456 0.036 Uiso 1 1 calc R
H20N H 0.325760 0.280383 0.707265 0.036 Uiso 1 1 calc R
C208 C 0.3128(4) 0.1474(3) 0.67832(16) 0.0291(9) Uani 1 1 d .
H20O H 0.383276 0.139569 0.709017 0.035 Uiso 1 1 calc R
H20P H 0.240473 0.097333 0.668568 0.035 Uiso 1 1 calc R
C209 C 0.4354(4) 0.0789(2) 0.60939(16) 0.0268(9) Uani 1 1 d .
H20Q H 0.364644 0.028408 0.592934 0.032 Uiso 1 1 calc R
H20R H 0.496892 0.065982 0.641128 0.032 Uiso 1 1 calc R
C210 C 0.5164(4) 0.0971(2) 0.56461(16) 0.0248(8) Uani 1 1 d .
H21A H 0.583679 0.149344 0.580703 0.030 Uiso 1 1 calc R
H21B H 0.566412 0.048311 0.552952 0.030 Uiso 1 1 calc R
C211 C 0.5039(3) 0.1341(2) 0.47524(15) 0.0245(9) Uani 1 1 d .
H21C H 0.568871 0.092918 0.466837 0.029 Uiso 1 1 calc R
H21D H 0.556373 0.192031 0.491307 0.029 Uiso 1 1 calc R
C212 C 0.4054(4) 0.1344(2) 0.42088(16) 0.0255(9) Uani 1 1 d .
H21E H 0.458404 0.138334 0.390878 0.031 Uiso 1 1 calc R
H21F H 0.343515 0.079229 0.408727 0.031 Uiso 1 1 calc R
C213 C 0.0151(3) 0.1822(3) 0.64836(15) 0.0277(9) Uani 1 1 d .
H21G H -0.031802 0.202009 0.680013 0.033 Uiso 1 1 calc R
H21H H 0.043513 0.125971 0.651531 0.033 Uiso 1 1 calc R
C214 C -0.0857(4) 0.1699(3) 0.59287(16) 0.0292(9) Uani 1 1 d .
H21I H -0.167829 0.130524 0.593014 0.035 Uiso 1 1 calc R
H21J H -0.113906 0.225828 0.588854 0.035 Uiso 1 1 calc R
C215 C -0.1243(4) 0.1102(3) 0.49347(15) 0.0271(9) Uani 1 1 d .
H21K H -0.166421 0.161095 0.486883 0.033 Uiso 1 1 calc R
H21L H -0.196837 0.066027 0.496574 0.033 Uiso 1 1 calc R
C216 C -0.0561(4) 0.0749(2) 0.44435(16) 0.0277(9) Uani 1 1 d .
H21M H -0.010401 0.025533 0.451655 0.033 Uiso 1 1 calc R
H21N H -0.125281 0.054655 0.409367 0.033 Uiso 1 1 calc R
C217 C 0.0917(4) 0.1158(3) 0.38543(16) 0.0315(10) Uani 1 1 d .
H21O H 0.014915 0.105073 0.353139 0.038 Uiso 1 1 calc R
H21P H 0.131667 0.061861 0.384871 0.038 Uiso 1 1 calc R
C218 C 0.1996(4) 0.1870(3) 0.38051(16) 0.0299(9) Uani 1 1 d .
H21Q H 0.229771 0.169615 0.344098 0.036 Uiso 1 1 calc R
H21R H 0.157480 0.240078 0.380265 0.036 Uiso 1 1 calc R
K201 K 0.23408(8) 0.22757(5) 0.54014(3) 0.02389(19) Uani 1 1 d .
N201 N 0.1398(3) 0.2455(2) 0.65392(13) 0.0253(7) Uani 1 1 d .
N202 N 0.3222(3) 0.2067(2) 0.42731(13) 0.0247(7) Uani 1 1 d .
O201 O 0.2373(3) 0.39321(16) 0.60907(11) 0.0321(6) Uani 1 1 d .
O202 O 0.3641(2) 0.38135(17) 0.51142(11) 0.0307(6) Uani 1 1 d .
O203 O 0.3725(2) 0.15370(16) 0.62937(10) 0.0257(6) Uani 1 1 d .
O204 O 0.4254(2) 0.10922(16) 0.51598(10) 0.0249(6) Uani 1 1 d .
O205 O -0.0228(2) 0.13423(16) 0.54575(10) 0.0244(6) Uani 1 1 d .
O206 O 0.0432(2) 0.14232(16) 0.43772(10) 0.0262(6) Uani 1 1 d .
C301 C 1.1097(3) 0.4981(2) 0.38877(15) 0.0190(8) Uani 1 1 d .
C302 C 0.9518(3) 0.3738(2) 0.38247(15) 0.0200(8) Uani 1 1 d .
C303 C 0.8758(3) 0.2918(2) 0.35138(15) 0.0202(8) Uani 1 1 d .
C304 C 0.7861(4) 0.1689(2) 0.28383(16) 0.0262(9) Uani 1 1 d .
H304 H 0.778333 0.132983 0.247327 0.031 Uiso 1 1 calc R
C305 C 0.7072(4) 0.1402(2) 0.32100(16) 0.0260(9) Uani 1 1 d .
H305 H 0.649193 0.086866 0.307626 0.031 Uiso 1 1 calc R
C306 C 0.7956(3) 0.2619(2) 0.38941(15) 0.0205(8) Uani 1 1 d .
C307 C 0.8296(3) 0.3272(2) 0.44183(15) 0.0200(8) Uani 1 1 d .
C308 C 0.8004(3) 0.3783(2) 0.53752(15) 0.0198(8) Uani 1 1 d .
C309 C 0.7331(3) 0.3736(2) 0.58663(15) 0.0191(8) Uani 1 1 d .
C310 C 0.5977(4) 0.3254(2) 0.64210(16) 0.0272(9) Uani 1 1 d .
H310 H 0.530769 0.284496 0.648498 0.033 Uiso 1 1 calc R
C311 C 0.6521(4) 0.3983(2) 0.68605(16) 0.0268(9) Uani 1 1 d .
H311 H 0.619546 0.403576 0.720392 0.032 Uiso 1 1 calc R
C312 C 0.7873(3) 0.4470(2) 0.63087(15) 0.0192(8) Uani 1 1 d .
N301 N 1.1055(3) 0.54509(18) 0.44426(12) 0.0210(7) Uani 1 1 d .
H301 H 1.050111 0.528159 0.465035 0.025 Uiso 1 1 calc R
N302 N 1.0431(3) 0.42308(19) 0.35989(12) 0.0209(7) Uani 1 1 d .
N303 N 0.9238(3) 0.39437(18) 0.43716(12) 0.0195(6) Uani 1 1 d .
N304 N 0.8722(3) 0.24466(19) 0.29729(13) 0.0244(7) Uani 1 1 d .
N305 N 0.7103(3) 0.18487(19) 0.37462(13) 0.0255(7) Uani 1 1 d .
N306 N 0.7703(3) 0.32082(19) 0.48897(12) 0.0219(7) Uani 1 1 d .
N307 N 0.6363(3) 0.31069(19) 0.59081(13) 0.0256(7) Uani 1 1 d .
N308 N 0.7490(3) 0.46180(19) 0.68217(13) 0.0249(7) Uani 1 1 d .
C401 C 0.6862(3) 0.3959(2) 1.06263(15) 0.0172(7) Uani 1 1 d .
C402 C 0.5629(3) 0.3145(2) 0.97236(15) 0.0188(8) Uani 1 1 d .
C403 C 0.5291(3) 0.2346(2) 0.92963(15) 0.0181(8) Uani 1 1 d .
C404 C 0.5163(4) 0.0956(2) 0.87974(16) 0.0257(9) Uani 1 1 d .
H404 H 0.542818 0.039925 0.875283 0.031 Uiso 1 1 calc R
C405 C 0.4187(4) 0.1119(2) 0.83556(16) 0.0266(9) Uani 1 1 d .
H405 H 0.383495 0.065919 0.803767 0.032 Uiso 1 1 calc R
C406 C 0.4309(3) 0.2511(2) 0.88443(15) 0.0198(8) Uani 1 1 d .
C407 C 0.4105(3) 0.3401(2) 0.90201(15) 0.0186(8) Uani 1 1 d .
C408 C 0.3037(3) 0.4608(2) 0.88497(15) 0.0193(8) Uani 1 1 d .
C409 C 0.2094(3) 0.5062(2) 0.85195(15) 0.0188(8) Uani 1 1 d .
C410 C 0.0599(4) 0.5338(2) 0.78043(17) 0.0289(9) Uani 1 1 d .
H410 H 0.003496 0.516695 0.744197 0.035 Uiso 1 1 calc R
C411 C 0.0654(4) 0.6193(3) 0.81138(17) 0.0304(9) Uani 1 1 d .
H411 H 0.013207 0.656543 0.794823 0.036 Uiso 1 1 calc R
C412 C 0.2152(3) 0.5917(2) 0.88354(15) 0.0189(8) Uani 1 1 d .
N401 N 0.6360(3) 0.47587(18) 1.06501(12) 0.0180(6) Uani 1 1 d .
H401 H 0.574281 0.485339 1.038449 0.022 Uiso 1 1 calc R
N402 N 0.6562(3) 0.32392(18) 1.02301(12) 0.0197(7) Uani 1 1 d .
N403 N 0.4909(3) 0.37735(18) 0.95529(12) 0.0196(7) Uani 1 1 d .
N404 N 0.5729(3) 0.15575(19) 0.92776(13) 0.0234(7) Uani 1 1 d .
N405 N 0.3733(3) 0.18887(19) 0.83621(13) 0.0244(7) Uani 1 1 d .
N406 N 0.3213(3) 0.37963(19) 0.86891(12) 0.0217(7) Uani 1 1 d .
N407 N 0.1312(3) 0.47410(19) 0.79960(13) 0.0256(7) Uani 1 1 d .
N408 N 0.1429(3) 0.6508(2) 0.86436(13) 0.0266(7) Uani 1 1 d .
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0125
0 1 0 0.0265
0 0 1 0.0312
0 0 -1 0.0312
-5 1 2 0.2280
5 -1 -2 0.2651
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
C52 C51 Cl51 121.3(3) . .
C56 C51 C52 119.5(4) . .
C56 C51 Cl51 119.2(3) . .
C51 C52 Cl52 120.6(3) . .
C53 C52 C51 120.3(4) . .
C53 C52 Cl52 119.1(3) . .
C54 C53 C52 119.6(4) . .
C53 C54 C55 120.4(4) . .
C56 C55 C54 120.0(4) . .
C55 C56 C51 120.1(4) . .
N101 C101 C102 113.0(4) . .
O101 C102 C101 109.2(3) . .
O101 C103 C104 109.6(3) . .
O102 C104 C103 109.9(3) . .
O102 C105 C106 110.0(3) . .
N102 C106 C105 113.3(3) . .
N101 C107 C108 114.8(3) . .
O103 C108 C107 110.4(4) . .
O103 C109 C110 109.1(3) . .
O104 C110 C109 109.6(3) . .
O104 C111 C112 109.4(3) . .
N102 C112 C111 113.7(3) . .
N101 C113 C114 113.8(3) . .
O105 C114 C113 109.6(3) . .
O105 C115 C116 109.2(3) . .
O106 C116 C115 109.6(3) . .
O106 C117 C118 108.4(3) . .
N102 C118 C117 112.6(3) . .
N102 K101 N101 179.82(9) . .
O101 K101 N101 59.40(8) . .
O101 K101 N102 120.43(8) . .
O102 K101 N101 118.69(8) . .
O102 K101 N102 61.13(8) . .
O102 K101 O101 60.64(7) . .
O102 K101 O103 119.99(7) . .
O102 K101 O104 100.46(8) . .
O102 K101 O105 128.15(8) . .
O102 K101 O106 89.99(7) . .
O103 K101 N101 60.56(9) . .
O103 K101 N102 119.46(9) . .
O103 K101 O101 99.48(8) . .
O103 K101 O104 60.00(9) . .
O103 K101 O106 147.24(8) . .
O104 K101 N101 119.31(9) . .
O104 K101 N102 60.76(8) . .
O104 K101 O101 142.43(7) . .
O105 K101 N101 59.03(7) . .
O105 K101 N102 121.09(8) . .
O105 K101 O101 86.74(7) . .
O105 K101 O103 103.28(8) . .
O105 K101 O104 126.65(7) . .
O105 K101 O106 60.79(7) . .
O106 K101 N101 118.72(8) . .
O106 K101 N102 61.37(7) . .
O106 K101 O101 107.33(7) . .
O106 K101 O104 104.59(8) . .
C101 N101 C107 110.3(3) . .
C101 N101 C113 111.0(3) . .
C101 N101 K101 110.6(2) . .
C107 N101 K101 107.8(2) . .
C113 N101 C107 110.2(3) . .
C113 N101 K101 107.0(2) . .
C106 N102 K101 108.3(2) . .
C112 N102 C106 110.6(3) . .
C112 N102 K101 109.3(2) . .
C118 N102 C106 110.2(3) . .
C118 N102 C112 108.4(3) . .
C118 N102 K101 109.9(2) . .
C102 O101 C103 110.1(3) . .
C102 O101 K101 115.7(2) . .
C103 O101 K101 112.4(2) . .
C104 O102 C105 110.6(3) . .
C104 O102 K101 115.0(2) . .
C105 O102 K101 119.66(19) . .
C108 O103 C109 111.3(3) . .
C108 O103 K101 118.4(2) . .
C109 O103 K101 116.1(2) . .
C110 O104 C111 111.2(3) . .
C110 O104 K101 110.8(2) . .
C111 O104 K101 116.0(2) . .
C114 O105 C115 111.5(3) . .
C114 O105 K101 125.29(19) . .
C115 O105 K101 114.35(19) . .
C116 O106 C117 111.3(3) . .
C116 O106 K101 113.56(19) . .
C117 O106 K101 110.08(18) . .
N201 C201 C202 114.9(3) . .
O201 C202 C201 108.8(3) . .
O201 C203 C204 107.8(3) . .
O202 C204 C203 109.8(3) . .
O202 C205 C206 108.7(3) . .
N202 C206 C205 113.3(3) . .
N201 C207 C208 113.0(3) . .
O203 C208 C207 108.7(3) . .
O203 C209 C210 108.8(3) . .
O204 C210 C209 110.3(3) . .
O204 C211 C212 109.1(3) . .
N202 C212 C211 113.4(3) . .
N201 C213 C214 113.8(3) . .
O205 C214 C213 110.0(3) . .
O205 C215 C216 109.5(3) . .
O206 C216 C215 109.1(3) . .
O206 C217 C218 109.1(3) . .
N202 C218 C217 113.7(3) . .
N202 K201 N201 178.80(8) . .
O201 K201 N201 60.20(8) . .
O201 K201 N202 120.77(8) . .
O201 K201 O202 59.84(7) . .
O201 K201 O203 96.41(8) . .
O201 K201 O204 137.57(8) . .
O201 K201 O205 103.93(7) . .
O201 K201 O206 127.86(8) . .
O202 K201 N201 119.45(8) . .
O202 K201 N202 61.63(8) . .
O203 K201 N201 58.91(8) . .
O203 K201 N202 121.21(8) . .
O203 K201 O202 121.30(7) . .
O204 K201 N201 117.39(8) . .
O204 K201 N202 62.49(8) . .
O204 K201 O202 100.94(7) . .
O204 K201 O203 59.54(7) . .
O204 K201 O205 109.83(7) . .
O204 K201 O206 91.86(7) . .
O205 K201 N201 60.22(7) . .
O205 K201 N202 118.62(8) . .
O205 K201 O202 144.71(8) . .
O205 K201 O203 89.83(7) . .
O205 K201 O206 59.66(7) . .
O206 K201 N201 118.96(7) . .
O206 K201 N202 59.95(7) . .
O206 K201 O202 103.52(7) . .
O206 K201 O203 129.37(7) . .
C201 N201 C207 110.5(3) . .
C201 N201 C213 109.3(3) . .
C201 N201 K201 106.7(2) . .
C207 N201 K201 109.99(19) . .
C213 N201 C207 109.9(3) . .
C213 N201 K201 110.4(2) . .
C206 N202 K201 108.9(2) . .
C212 N202 C206 109.8(3) . .
C212 N202 C218 110.0(3) . .
C212 N202 K201 108.1(2) . .
C218 N202 C206 109.8(3) . .
C218 N202 K201 110.21(19) . .
C202 O201 C203 112.5(3) . .
C202 O201 K201 122.6(2) . .
C203 O201 K201 118.7(2) . .
C204 O202 K201 109.5(2) . .
C205 O202 C204 110.9(3) . .
C205 O202 K201 110.9(2) . .
C208 O203 K201 120.9(2) . .
C209 O203 C208 112.2(3) . .
C209 O203 K201 114.8(2) . .
C210 O204 C211 110.3(2) . .
C210 O204 K201 115.54(19) . .
C211 O204 K201 110.2(2) . .
C214 O205 C215 110.2(3) . .
C214 O205 K201 116.01(19) . .
C215 O205 K201 116.11(18) . .
C216 O206 K201 114.5(2) . .
C217 O206 C216 110.3(3) . .
C217 O206 K201 119.99(19) . .
N301 C301 C312 104.4(3) . 2_766
N302 C301 C312 125.6(3) . 2_766
N302 C301 N301 130.0(3) . .
N302 C302 C303 123.2(3) . .
N303 C302 C303 110.4(3) . .
N303 C302 N302 126.4(3) . .
C302 C303 C306 106.1(3) . .
N304 C303 C302 131.5(3) . .
N304 C303 C306 122.4(3) . .
N304 C304 C305 124.3(3) . .
N305 C305 C304 123.7(3) . .
C307 C306 C303 105.9(3) . .
N305 C306 C303 123.0(3) . .
N305 C306 C307 131.0(3) . .
N303 C307 C306 110.3(3) . .
N303 C307 N306 127.3(3) . .
N306 C307 C306 122.4(3) . .
N301 C308 C309 104.8(3) 2_766 .
N306 C308 C309 124.0(3) . .
N306 C308 N301 131.2(3) . 2_766
C312 C309 C308 108.7(3) . .
N307 C309 C308 127.8(3) . .
N307 C309 C312 123.5(3) . .
N307 C310 C311 123.4(3) . .
N308 C311 C310 124.0(3) . .
C309 C312 C301 108.6(3) . 2_766
N308 C312 C301 127.7(3) . 2_766
N308 C312 C309 123.7(3) . .
C308 N301 C301 113.4(3) 2_766 .
C301 N302 C302 122.0(3) . .
C307 N303 C302 107.2(3) . .
C304 N304 C303 113.1(3) . .
C305 N305 C306 113.5(3) . .
C308 N306 C307 124.0(3) . .
C309 N307 C310 113.0(3) . .
C312 N308 C311 112.5(3) . .
N401 C401 C412 105.1(3) . 2_667
N402 C401 C412 124.8(3) . 2_667
N402 C401 N401 130.1(3) . .
N402 C402 C403 122.8(3) . .
N403 C402 C403 110.1(3) . .
N403 C402 N402 127.0(3) . .
C402 C403 C406 106.1(3) . .
N404 C403 C402 131.2(3) . .
N404 C403 C406 122.7(3) . .
N404 C404 C405 123.6(3) . .
N405 C405 C404 124.3(3) . .
C407 C406 C403 106.2(3) . .
N405 C406 C403 122.9(3) . .
N405 C406 C407 130.9(3) . .
N403 C407 C406 109.9(3) . .
N403 C407 N406 127.3(3) . .
N406 C407 C406 122.8(3) . .
N401 C408 C409 104.6(3) 2_667 .
N406 C408 C409 125.1(3) . .
N406 C408 N401 130.4(3) . 2_667
C412 C409 C408 108.7(3) . .
N407 C409 C408 127.5(3) . .
N407 C409 C412 123.8(3) . .
N407 C410 C411 124.0(4) . .
N408 C411 C410 123.0(4) . .
C409 C412 C401 108.6(3) . 2_667
N408 C412 C401 128.2(3) . 2_667
N408 C412 C409 123.2(3) . .
C401 N401 C408 113.1(3) . 2_667
C401 N402 C402 123.4(3) . .
C402 N403 C407 107.7(3) . .
C404 N404 C403 113.6(3) . .
C405 N405 C406 113.0(3) . .
C408 N406 C407 122.6(3) . .
C409 N407 C410 112.7(3) . .
C412 N408 C411 113.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C51 C52 1.391(5) .
C51 C56 1.386(6) .
C51 Cl51 1.730(4) .
C52 C53 1.385(5) .
C52 Cl52 1.731(4) .
C53 C54 1.379(6) .
C54 C55 1.385(6) .
C55 C56 1.380(6) .
C101 C102 1.506(5) .
C101 N101 1.465(5) .
C102 O101 1.422(4) .
C103 C104 1.491(5) .
C103 O101 1.427(4) .
C104 O102 1.418(4) .
C105 C106 1.502(5) .
C105 O102 1.426(4) .
C106 N102 1.475(4) .
C107 C108 1.499(6) .
C107 N101 1.476(5) .
C108 O103 1.413(5) .
C109 C110 1.480(6) .
C109 O103 1.425(5) .
C110 O104 1.419(4) .
C111 C112 1.499(5) .
C111 O104 1.425(5) .
C112 N102 1.472(5) .
C113 C114 1.509(5) .
C113 N101 1.471(4) .
C114 O105 1.420(4) .
C115 C116 1.495(5) .
C115 O105 1.430(4) .
C116 O106 1.426(4) .
C117 C118 1.506(5) .
C117 O106 1.432(4) .
C118 N102 1.470(4) .
K101 N101 3.043(3) .
K101 N102 2.963(3) .
K101 O101 2.877(3) .
K101 O102 2.773(2) .
K101 O103 2.812(3) .
K101 O104 2.874(3) .
K101 O105 2.775(2) .
K101 O106 2.848(2) .
C201 C202 1.505(5) .
C201 N201 1.472(5) .
C202 O201 1.415(4) .
C203 C204 1.487(5) .
C203 O201 1.429(4) .
C204 O202 1.432(4) .
C205 C206 1.509(5) .
C205 O202 1.429(4) .
C206 N202 1.477(4) .
C207 C208 1.513(5) .
C207 N201 1.479(5) .
C208 O203 1.424(4) .
C209 C210 1.505(5) .
C209 O203 1.417(4) .
C210 O204 1.421(4) .
C211 C212 1.506(5) .
C211 O204 1.442(4) .
C212 N202 1.465(4) .
C213 C214 1.501(5) .
C213 N201 1.473(4) .
C214 O205 1.424(4) .
C215 C216 1.493(5) .
C215 O205 1.436(4) .
C216 O206 1.424(4) .
C217 C218 1.504(5) .
C217 O206 1.421(4) .
C218 N202 1.475(4) .
K201 N201 3.016(3) .
K201 N202 2.964(3) .
K201 O201 2.777(3) .
K201 O202 2.895(3) .
K201 O203 2.886(3) .
K201 O204 2.822(3) .
K201 O205 2.835(2) .
K201 O206 2.841(3) .
C301 C312 1.470(4) 2_766
C301 N301 1.400(4) .
C301 N302 1.289(4) .
C302 C303 1.417(5) .
C302 N302 1.383(4) .
C302 N303 1.375(4) .
C303 C306 1.429(4) .
C303 N304 1.356(4) .
C304 C305 1.397(5) .
C304 N304 1.340(4) .
C305 N305 1.334(4) .
C306 C307 1.422(5) .
C306 N305 1.350(4) .
C307 N303 1.373(4) .
C307 N306 1.382(4) .
C308 C309 1.465(4) .
C308 N301 1.389(4) 2_766
C308 N306 1.293(4) .
C309 C312 1.392(5) .
C309 N307 1.337(4) .
C310 C311 1.383(5) .
C310 N307 1.339(4) .
C311 N308 1.341(4) .
C312 N308 1.338(4) .
C401 C412 1.460(5) 2_667
C401 N401 1.392(4) .
C401 N402 1.293(4) .
C402 C403 1.421(5) .
C402 N402 1.380(4) .
C402 N403 1.369(4) .
C403 C406 1.426(5) .
C403 N404 1.350(4) .
C404 C405 1.404(5) .
C404 N404 1.334(4) .
C405 N405 1.331(4) .
C406 C407 1.420(5) .
C406 N405 1.355(4) .
C407 N403 1.376(4) .
C407 N406 1.379(4) .
C408 C409 1.466(5) .
C408 N401 1.397(4) 2_667
C408 N406 1.292(4) .
C409 C412 1.392(5) .
C409 N407 1.339(4) .
C410 C411 1.386(5) .
C410 N407 1.343(5) .
C411 N408 1.347(5) .
C412 N408 1.341(4) .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0001 -0.9997 -0.0000 -0.0007 0.0427 0.0184
0.0001 0.9997 0.0000 0.0007 -0.0427 -0.0184
0.0001 0.0001 0.9993 -0.0295 -0.0072 -0.0024
-0.0001 -0.0001 -0.9993 0.0295 0.0072 0.0024
-4.9972 0.9987 1.9983 0.0079 -0.1509 0.3266
4.9972 -0.9987 -1.9983 -0.0079 0.1509 -0.3266
