#------------------------------------------------------------------------------
#$Date: 2022-09-06 19:18:56 +0300 (Tue, 06 Sep 2022) $
#$Revision: 277687 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/75/1567588.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_1567588
loop_
_publ_author_name
'Rocco, Dalila'
'Nikoletić, Anamarija'
'Prescimone, Alessandro'
'Constable, Edwin C.'
'Housecroft, Catherine E.'
_publ_section_title
;
 To Be or Not to Be a (4,4) Net: Reactions of
 4′-{4-(N,N-Diethylaminophenyl)}- and
 4′-{4-(N,N-Diphenylaminophenyl)}-3,2′:6′,3″-
 and 4,2′:6′,4″-Terpyridines with Cobalt(II)
 Thiocyanate
;
_journal_issue                   8
_journal_name_full               Crystals
_journal_page_first              1136
_journal_paper_doi               10.3390/cryst12081136
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C52 H50 Co N10 S2, 0.8(C H Cl3)'
_chemical_formula_sum            'C52.8 H48.8 Cl2.4 Co N10 S2'
_chemical_formula_weight         1031.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.533(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3183(3)
_cell_length_b                   12.5045(2)
_cell_length_c                   15.2418(4)
_cell_measurement_reflns_used    39015
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.99
_cell_measurement_theta_min      3.34
_cell_volume                     2521.87(10)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
 1957 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Basel-Cu-Stoe
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22004
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.668
_diffrn_reflns_theta_min         4.179
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.982
_exptl_absorpt_correction_T_max  0.0628
_exptl_absorpt_correction_T_min  0.0325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1071
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of CHCl3 and methanol  by solvent layering'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.16
_exptl_crystal_size_rad          0.200
_refine_diff_density_max         1.936
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0029(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.1030
_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)+(0.1000P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2365
_refine_ls_wR_factor_ref         0.2400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4678
_reflns_number_total             4963
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            NIA003_150K.cif
_cod_data_source_block           nia003_150k
_cod_original_formula_sum        'C52.80 H48.80 Cl2.40 Co N10 S2'
_cod_database_code               1567588
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.407
_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. Restrained distances
 N4-C24 \\sim N5-C24 \\sim N5-C22 \\sim N4-C26 \\sim N5-C19 \\sim N4-C19
 with sigma of 0.02
 C27-C26 \\sim C22-C23 \\sim C25-C24
 with sigma of 0.02
 C29-Cl1 \\sim C29-Cl3 \\sim C29-Cl2
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl3-Cl2
 with sigma of 0.04
 N4-C19 \\sim N4-C24 \\sim N4-C26
 with sigma of 0.02
 N5-C19 \\sim N5-C24 \\sim N5-C22
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C29) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl2) = Uanis(Cl1) = Uanis(Cl3)
4. Rigid body (RIGU) restrains
 C23, C27, C22, C26, C25, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C5, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C1(0.55) H1(0.55) C3(0.55) H3(0.55) N5(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) H24D(0.5) C2(0.55) H2(0.55) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5) Cl1(0.4) N4(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C22(0.5) H22A(0.5) H22B(0.5) C29(0.4) H29(0.4) Cl3(0.4) Cl2(0.4)
 C31(0.45) H31(0.45) C30(0.45) H30(0.45) C32(0.45) H32(0.45)
6.a Riding coordinates:
 C1(H1), C3(H3), C24(H24C,H24D), C2(H2), C31(H31), C30(H30), C32(H32)
6.b Ternary CH refined with riding coordinates:
 C29(H29)
6.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C22(H22A,H22B)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C5(H5), C12(H12), C7(H7), C17(H17), C15(H15), C13(H13), C21(H21),
 C14(H14), C18(H18), C20(H20)
6.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C)
;
_olex2_date_sample_data_collection 2022-05-09
_olex2_date_sample_submission    2022-04-12
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id NIA003_150K
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   6.5
_stoe_evaluation_integration_b   -0.4
_stoe_evaluation_integration_ems 0.017
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 98.8
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 145.4
_stoe_evaluation_lana_max_2theta_desired 145.4
_stoe_evaluation_lana_mean_redundancy 4.4
_stoe_evaluation_lana_number_refls_after_or 22009
_stoe_evaluation_lana_number_refls_outliers 8743
_stoe_evaluation_lana_number_refls_total 30752
_stoe_evaluation_lana_number_refls_unique 4966
_stoe_evaluation_lana_number_refls_written 22009
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
----------------------------------------------------------------------------
2Theta          13.2   28.8   44.4   60.0   75.6   91.2  106.8  122.4  138.0
----------------------------------------------------------------------------
<Resolution>    5.33   2.96   2.01   1.50   1.26   1.08   0.96   0.88   0.83
N(total)          76    506   1529   3524   6544   6903   4872   4467   2331
<Redundancy>     1.9    2.6    3.3    4.9    6.6    6.1    3.9    3.6    2.6
Complet. [%%]    94.3   99.3  100.0   99.8  100.0  100.0   99.9   99.9   92.5
<I/sigma>      610.7  299.5  152.0   71.7   45.1   29.6   22.3   16.8   12.1
R(int)         0.022  0.021  0.027  0.027  0.029  0.030  0.040  0.069  0.145
----------------------------------------------------------------------------
;
_stoe_measurement_identifier     NIA003_150K
_stoe_measurement_max_exposure_per_frame '8.0 s'
_stoe_measurement_mean_exposure_per_frame '7.6 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '4.2 h'
_stoe_measurement_total_frame_number 1957
_stoe_measurement_total_run_number 35
_stoe_measurement_tube_power     '50.0 W'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Co1 Co 0.000000 1.000000 0.500000 0.0309(3) Uani 1 2 d S . P A .
S1 S -0.04223(14) 0.76731(14) 0.74443(9) 0.0624(5) Uani 1 1 d . . . . .
N6 N -0.0250(3) 0.8814(3) 0.5905(2) 0.0357(9) Uani 1 1 d . . . . .
N3 N 0.3853(3) 0.5712(3) 0.9008(2) 0.0373(9) Uani 1 1 d . . . . .
N1 N 0.1163(3) 0.8999(3) 0.4484(2) 0.0395(9) Uani 1 1 d . . . . .
N2 N 0.2679(3) 0.6633(3) 0.6027(3) 0.0386(9) Uani 1 1 d . . . . .
C28 C -0.0328(3) 0.8328(4) 0.6543(3) 0.0342(10) Uani 1 1 d . . . . .
C8 C 0.3367(4) 0.4742(4) 0.5287(3) 0.0367(10) Uani 1 1 d . . . . .
C9 C 0.3472(4) 0.4906(4) 0.6199(3) 0.0396(11) Uani 1 1 d . . . . .
H9 H 0.378971 0.439219 0.657505 0.048 Uiso 1 1 calc R U . . .
C16 C 0.3692(4) 0.3740(4) 0.4883(3) 0.0387(11) Uani 1 1 d . . . . .
C5 C 0.1558(4) 0.8148(4) 0.4931(3) 0.0362(10) Uani 1 1 d . . . . .
H5 H 0.138219 0.803536 0.549744 0.043 Uiso 1 1 calc R U . . .
C11 C 0.3109(4) 0.6034(4) 0.7505(3) 0.0424(12) Uani 1 1 d . . . . .
C12 C 0.3818(4) 0.5558(4) 0.8124(3) 0.0418(11) Uani 1 1 d . . . . .
H12 H 0.429626 0.510817 0.791976 0.050 Uiso 1 1 calc R U . . .
C7 C 0.2926(4) 0.5572(4) 0.4758(3) 0.0385(11) Uani 1 1 d . . . . .
H7 H 0.284006 0.549913 0.414685 0.046 Uiso 1 1 calc R U . . .
C10 C 0.3101(4) 0.5837(4) 0.6544(3) 0.0386(11) Uani 1 1 d . . . . .
C6 C 0.2616(4) 0.6502(4) 0.5144(3) 0.0374(10) Uani 1 1 d . . . . .
C17 C 0.4608(4) 0.3264(4) 0.5174(3) 0.0436(12) Uani 1 1 d . . . . .
H17 H 0.502521 0.358316 0.563053 0.052 Uiso 1 1 calc R U . . .
C4 C 0.2213(4) 0.7422(4) 0.4608(3) 0.0421(12) Uani 1 1 d . . . . .
C15 C 0.3143(4) 0.6350(5) 0.9281(3) 0.0481(13) Uani 1 1 d . . . . .
H15 H 0.314710 0.646576 0.988438 0.058 Uiso 1 1 calc R U . . .
C13 C 0.2399(5) 0.6701(5) 0.7811(3) 0.0506(14) Uani 1 1 d . . . . .
H13 H 0.192287 0.704967 0.741730 0.061 Uiso 1 1 calc R U . . .
C21 C 0.3068(4) 0.3217(5) 0.4222(4) 0.0536(14) Uani 1 1 d . . . . .
H21 H 0.244966 0.351733 0.400696 0.064 Uiso 1 1 calc R U . . .
C14 C 0.2405(5) 0.6844(5) 0.8711(3) 0.0550(15) Uani 1 1 d . . . . .
H14 H 0.191779 0.726869 0.893097 0.066 Uiso 1 1 calc R U . . .
C18 C 0.4916(5) 0.2338(5) 0.4808(4) 0.0511(13) Uani 1 1 d . . . . .
H18 H 0.554983 0.205905 0.500303 0.061 Uiso 1 1 calc R U . . .
C19 C 0.4299(5) 0.1805(5) 0.4149(5) 0.0663(18) Uani 1 1 d D . . . .
C20 C 0.3360(5) 0.2260(6) 0.3884(5) 0.074(2) Uani 1 1 d . . . . .
H20 H 0.291574 0.190638 0.346649 0.089 Uiso 1 1 calc R U . . .
C1 C 0.1273(10) 0.9051(11) 0.3629(8) 0.040(3) Uani 0.55 1 d . . P A 1
H1 H 0.096060 0.960659 0.329548 0.048 Uiso 0.55 1 d R U P A 1
C3 C 0.2331(10) 0.7510(13) 0.3724(10) 0.038(3) Uani 0.55 1 d . . P A 1
H3 H 0.271970 0.700846 0.346407 0.046 Uiso 0.55 1 d R U P A 1
N5 N 0.4613(9) 0.0938(10) 0.3590(7) 0.066(4) Uani 0.5 1 d D . P B 1
C24 C 0.5568(6) 0.0383(6) 0.4007(6) 0.080(2) Uani 1 1 d D . . . .
H24A H 0.569758 0.053772 0.463319 0.096 Uiso 0.5 1 calc R U P B 1
H24B H 0.553075 -0.038473 0.392035 0.096 Uiso 0.5 1 calc R U P B 1
H24C H 0.585491 0.041290 0.462076 0.096 Uiso 0.5 1 d R U P B 2
H24D H 0.552481 -0.035560 0.381316 0.096 Uiso 0.5 1 d R U P B 2
C25 C 0.6349(7) 0.0878(7) 0.3502(6) 0.090(2) Uani 1 1 d D . . . .
H25A H 0.621501 0.068741 0.288997 0.136 Uiso 1 1 calc R U . . .
H25B H 0.700658 0.062271 0.373211 0.136 Uiso 1 1 calc R U . . .
H25C H 0.632732 0.164205 0.356067 0.136 Uiso 1 1 calc R U . . .
C2 C 0.1864(10) 0.8327(9) 0.3227(7) 0.045(2) Uani 0.55 1 d . . P A 1
H2 H 0.194451 0.839295 0.263078 0.054 Uiso 0.55 1 d R U P A 1
C26 C 0.3869(10) 0.0044(8) 0.3476(7) 0.052(3) Uani 0.5 1 d D . P B 2
H26A H 0.319384 0.014421 0.364284 0.062 Uiso 0.5 1 calc R U P B 2
H26B H 0.405720 -0.069525 0.359920 0.062 Uiso 0.5 1 calc R U P B 2
C27 C 0.3834(13) 0.0227(14) 0.2500(8) 0.072(4) Uani 0.5 1 d D . P B 2
H27A H 0.333965 -0.023817 0.219276 0.108 Uiso 0.5 1 calc R U P B 2
H27B H 0.448605 0.007812 0.231619 0.108 Uiso 0.5 1 calc R U P B 2
H27C H 0.365570 0.095743 0.236728 0.108 Uiso 0.5 1 calc R U P B 2
Cl1 Cl 0.4834(6) -0.0966(7) 0.0474(6) 0.0992(15) Uani 0.4 1 d D . P C -1
N4 N 0.4551(7) 0.0719(8) 0.4024(8) 0.049(3) Uani 0.5 1 d D . P B 2
C23 C 0.4599(16) 0.1569(14) 0.2005(11) 0.099(6) Uani 0.5 1 d D . P B 1
H23A H 0.426280 0.144125 0.142330 0.149 Uiso 0.5 1 calc R U P B 1
H23B H 0.531342 0.147099 0.200253 0.149 Uiso 0.5 1 calc R U P B 1
H23C H 0.446738 0.228825 0.218085 0.149 Uiso 0.5 1 calc R U P B 1
C22 C 0.4210(13) 0.0794(12) 0.2647(9) 0.078(4) Uani 0.5 1 d D . P B 1
H22A H 0.348003 0.085452 0.259715 0.094 Uiso 0.5 1 calc R U P B 1
H22B H 0.436957 0.007432 0.247029 0.094 Uiso 0.5 1 calc R U P B 1
C29 C 0.4875(14) 0.0345(11) 0.0264(9) 0.076(5) Uani 0.4 1 d D U P C -1
H29 H 0.427616 0.064464 0.049277 0.091 Uiso 0.4 1 calc R U P C -1
Cl3 Cl 0.4820(6) 0.0786(7) -0.0781(6) 0.0992(15) Uani 0.4 1 d D . P C -1
Cl2 Cl 0.5873(4) 0.0896(5) 0.0891(4) 0.0992(15) Uani 0.4 1 d D . P C -1
C31 C 0.2386(12) 0.8687(11) 0.3409(9) 0.047(3) Uani 0.45 1 d . . P A 2
H31 H 0.264974 0.888206 0.289230 0.056 Uiso 0.45 1 d R U P A 2
C30 C 0.1682(12) 0.9319(15) 0.3758(11) 0.043(4) Uani 0.45 1 d . . P A 2
H30 H 0.155558 0.999942 0.352560 0.052 Uiso 0.45 1 d R U P A 2
C32 C 0.2718(15) 0.7753(16) 0.3852(13) 0.048(4) Uani 0.45 1 d . . P A 2
H32 H 0.322084 0.732988 0.365537 0.058 Uiso 0.45 1 d R 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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
-2 1 30 0.0617
-11 -30 -21 0.1123
25 19 -30 0.0860
-21 13 30 0.0686
3 -10 7 0.1564
-30 -7 -25 0.1143
2 -1 -30 0.0402
30 1 26 0.0699
-9 -4 10 0.0786
3 -3 -5 0.0962
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
N6 Co1 N6 180.0 . 3_576 ?
N6 Co1 N3 89.07(15) 3_576 4_575 ?
N6 Co1 N3 90.93(15) . 4_575 ?
N6 Co1 N3 90.93(15) 3_576 2_556 ?
N6 Co1 N3 89.07(15) . 2_556 ?
N6 Co1 N1 90.20(15) . . ?
N6 Co1 N1 89.80(15) . 3_576 ?
N6 Co1 N1 90.20(15) 3_576 3_576 ?
N6 Co1 N1 89.80(15) 3_576 . ?
N3 Co1 N3 180.0 2_556 4_575 ?
N1 Co1 N3 90.79(16) . 2_556 ?
N1 Co1 N3 89.21(16) 3_576 2_556 ?
N1 Co1 N3 89.21(16) . 4_575 ?
N1 Co1 N3 90.79(16) 3_576 4_575 ?
N1 Co1 N1 180.00(18) . 3_576 ?
C28 N6 Co1 164.9(4) . . ?
C12 N3 Co1 124.4(3) . 2_546 ?
C15 N3 Co1 119.0(3) . 2_546 ?
C15 N3 C12 116.6(4) . . ?
C5 N1 Co1 121.4(3) . . ?
C5 N1 C30 114.9(8) . . ?
C1 N1 Co1 118.8(6) . . ?
C1 N1 C5 117.2(7) . . ?
C30 N1 Co1 122.6(8) . . ?
C6 N2 C10 117.8(4) . . ?
N6 C28 S1 178.7(5) . . ?
C9 C8 C16 122.4(4) . . ?
C9 C8 C7 116.9(4) . . ?
C7 C8 C16 120.7(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(5) . . ?
C10 C9 H9 120.0 . . ?
C17 C16 C8 121.3(5) . . ?
C17 C16 C21 117.5(5) . . ?
C21 C16 C8 121.2(5) . . ?
N1 C5 H5 117.8 . . ?
N1 C5 C4 124.4(4) . . ?
C4 C5 H5 117.8 . . ?
C12 C11 C10 121.8(4) . . ?
C13 C11 C12 117.9(5) . . ?
C13 C11 C10 120.3(5) . . ?
N3 C12 C11 123.9(5) . . ?
N3 C12 H12 118.1 . . ?
C11 C12 H12 118.1 . . ?
C8 C7 H7 119.9 . . ?
C6 C7 C8 120.1(4) . . ?
C6 C7 H7 119.9 . . ?
N2 C10 C9 122.6(4) . . ?
N2 C10 C11 114.1(4) . . ?
C9 C10 C11 123.3(4) . . ?
N2 C6 C7 122.5(4) . . ?
N2 C6 C4 115.8(4) . . ?
C7 C6 C4 121.7(4) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 C16 121.9(5) . . ?
C18 C17 H17 119.1 . . ?
C5 C4 C6 121.1(4) . . ?
C5 C4 C32 117.3(9) . . ?
C3 C4 C5 116.2(8) . . ?
C3 C4 C6 121.9(8) . . ?
C32 C4 C6 119.2(9) . . ?
N3 C15 H15 118.4 . . ?
N3 C15 C14 123.2(5) . . ?
C14 C15 H15 118.4 . . ?
C11 C13 H13 120.5 . . ?
C11 C13 C14 119.0(5) . . ?
C14 C13 H13 120.5 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.5(5) . . ?
C20 C21 H21 119.7 . . ?
C15 C14 C13 119.4(5) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C17 C18 H18 119.4 . . ?
C17 C18 C19 121.2(5) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 N5 126.0(7) . . ?
C18 C19 N4 115.2(7) . . ?
C20 C19 C18 116.8(5) . . ?
C20 C19 N5 116.0(7) . . ?
C20 C19 N4 124.8(7) . . ?
C21 C20 C19 122.0(6) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.1(11) . . ?
C2 C1 H1 119.2 . . ?
C4 C3 H3 119.5 . . ?
C2 C3 C4 120.2(13) . . ?
C2 C3 H3 120.3 . . ?
C19 N5 C24 111.9(8) . . ?
C19 N5 C22 123.7(10) . . ?
C22 N5 C24 122.7(10) . . ?
N5 C24 H24A 111.5 . . ?
N5 C24 H24B 111.5 . . ?
H24A C24 H24B 109.4 . . ?
H24C C24 H24D 109.4 . . ?
C25 C24 N5 101.2(8) . . ?
C25 C24 H24A 111.5 . . ?
C25 C24 H24B 111.5 . . ?
C25 C24 H24C 105.0 . . ?
C25 C24 H24D 104.9 . . ?
N4 C24 H24C 104.1 . . ?
N4 C24 H24D 105.3 . . ?
N4 C24 C25 127.4(8) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 119.0(11) . . ?
C3 C2 H2 120.5 . . ?
H26A C26 H26B 107.4 . . ?
C27 C26 H26A 108.4 . . ?
C27 C26 H26B 108.4 . . ?
N4 C26 H26A 108.4 . . ?
N4 C26 H26B 108.4 . . ?
N4 C26 C27 115.6(11) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C19 N4 C24 121.7(8) . . ?
C19 N4 C26 119.9(8) . . ?
C24 N4 C26 110.9(8) . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
N5 C22 C23 115.9(14) . . ?
N5 C22 H22A 108.3 . . ?
N5 C22 H22B 108.3 . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
Cl1 C29 H29 105.2 . . ?
Cl1 C29 Cl3 120.3(10) . . ?
Cl1 C29 Cl2 109.3(8) . . ?
Cl3 C29 H29 105.2 . . ?
Cl3 C29 Cl2 110.4(8) . . ?
Cl2 C29 H29 105.2 . . ?
C30 C31 H31 121.0 . . ?
C30 C31 C32 118.9(15) . . ?
C32 C31 H31 120.0 . . ?
N1 C30 H30 118.0 . . ?
C31 C30 N1 123.3(15) . . ?
C31 C30 H30 118.6 . . ?
C4 C32 H32 120.5 . . ?
C31 C32 C4 118.2(16) . . ?
C31 C32 H32 121.3 . . ?
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
Co1 N6 2.078(4) . ?
Co1 N6 2.078(4) 3_576 ?
Co1 N3 2.211(4) 4_575 ?
Co1 N3 2.211(4) 2_556 ?
Co1 N1 2.205(4) 3_576 ?
Co1 N1 2.205(4) . ?
S1 C28 1.616(5) . ?
N6 C28 1.162(6) . ?
N3 C12 1.357(6) . ?
N3 C15 1.339(7) . ?
N1 C5 1.339(6) . ?
N1 C1 1.330(13) . ?
N1 C30 1.427(17) . ?
N2 C10 1.352(6) . ?
N2 C6 1.349(6) . ?
C8 C9 1.396(7) . ?
C8 C16 1.483(7) . ?
C8 C7 1.401(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.391(7) . ?
C16 C17 1.383(7) . ?
C16 C21 1.394(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.388(7) . ?
C11 C12 1.390(7) . ?
C11 C10 1.485(6) . ?
C11 C13 1.382(7) . ?
C12 H12 0.9300 . ?
C7 H7 0.9300 . ?
C7 C6 1.386(7) . ?
C6 C4 1.476(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.369(8) . ?
C4 C3 1.379(17) . ?
C4 C32 1.46(2) . ?
C15 H15 0.9300 . ?
C15 C14 1.381(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.383(7) . ?
C21 H21 0.9300 . ?
C21 C20 1.376(8) . ?
C14 H14 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.393(9) . ?
C19 C20 1.392(9) . ?
C19 N5 1.469(10) . ?
C19 N4 1.417(10) . ?
C20 H20 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.387(17) . ?
C3 H3 0.9300 . ?
C3 C2 1.378(19) . ?
N5 C24 1.523(11) . ?
N5 C22 1.487(13) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9704 . ?
C24 H24D 0.9698 . ?
C24 C25 1.497(10) . ?
C24 N4 1.421(10) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C2 H2 0.9302 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.501(15) . ?
C26 N4 1.436(11) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Cl1 C29 1.672(12) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C23 C22 1.510(16) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C29 H29 0.9800 . ?
C29 Cl3 1.680(12) . ?
C29 Cl2 1.694(13) . ?
C31 H31 0.9299 . ?
C31 C30 1.38(2) . ?
C31 C32 1.40(2) . ?
C30 H30 0.9298 . ?
C32 H32 0.9302 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N3 C12 C11 -178.2(4) 2_546 . . . ?
Co1 N3 C15 C14 179.0(5) 2_546 . . . ?
Co1 N1 C5 C4 173.1(4) . . . . ?
Co1 N1 C1 C2 -169.1(10) . . . . ?
Co1 N1 C30 C31 -177.7(11) . . . . ?
N3 C15 C14 C13 -1.4(10) . . . . ?
N1 C5 C4 C6 -180.0(5) . . . . ?
N1 C5 C4 C3 -10.0(10) . . . . ?
N1 C5 C4 C32 17.6(11) . . . . ?
N1 C1 C2 C3 2(2) . . . . ?
N2 C6 C4 C5 -26.7(8) . . . . ?
N2 C6 C4 C3 163.9(8) . . . . ?
N2 C6 C4 C32 135.4(9) . . . . ?
C8 C9 C10 N2 -3.4(8) . . . . ?
C8 C9 C10 C11 175.0(5) . . . . ?
C8 C16 C17 C18 179.9(5) . . . . ?
C8 C16 C21 C20 -176.8(6) . . . . ?
C8 C7 C6 N2 -3.1(8) . . . . ?
C8 C7 C6 C4 175.8(5) . . . . ?
C9 C8 C16 C17 -44.0(8) . . . . ?
C9 C8 C16 C21 133.3(6) . . . . ?
C9 C8 C7 C6 0.0(8) . . . . ?
C16 C8 C9 C10 -176.3(5) . . . . ?
C16 C8 C7 C6 179.4(5) . . . . ?
C16 C17 C18 C19 -2.8(9) . . . . ?
C16 C21 C20 C19 -3.5(12) . . . . ?
C5 N1 C1 C2 -7.0(15) . . . . ?
C5 N1 C30 C31 14.1(17) . . . . ?
C5 C4 C3 C2 4.0(14) . . . . ?
C5 C4 C32 C31 -11.0(18) . . . . ?
C11 C13 C14 C15 2.4(10) . . . . ?
C12 N3 C15 C14 -0.4(9) . . . . ?
C12 C11 C10 N2 -154.6(5) . . . . ?
C12 C11 C10 C9 26.9(8) . . . . ?
C12 C11 C13 C14 -1.7(9) . . . . ?
C7 C8 C9 C10 3.1(8) . . . . ?
C7 C8 C16 C17 136.6(5) . . . . ?
C7 C8 C16 C21 -46.1(8) . . . . ?
C7 C6 C4 C5 154.4(5) . . . . ?
C7 C6 C4 C3 -15.0(10) . . . . ?
C7 C6 C4 C32 -43.5(11) . . . . ?
C10 N2 C6 C7 2.9(8) . . . . ?
C10 N2 C6 C4 -176.0(5) . . . . ?
C10 C11 C12 N3 -179.8(5) . . . . ?
C10 C11 C13 C14 178.1(6) . . . . ?
C6 N2 C10 C9 0.4(8) . . . . ?
C6 N2 C10 C11 -178.1(5) . . . . ?
C6 C4 C3 C2 173.9(9) . . . . ?
C6 C4 C32 C31 -173.7(12) . . . . ?
C17 C16 C21 C20 0.6(9) . . . . ?
C17 C18 C19 C20 0.0(11) . . . . ?
C17 C18 C19 N5 167.2(9) . . . . ?
C17 C18 C19 N4 -161.0(7) . . . . ?
C4 C3 C2 C1 -0.3(19) . . . . ?
C15 N3 C12 C11 1.1(8) . . . . ?
C13 C11 C12 N3 -0.1(9) . . . . ?
C13 C11 C10 N2 25.6(8) . . . . ?
C13 C11 C10 C9 -152.8(6) . . . . ?
C21 C16 C17 C18 2.5(8) . . . . ?
C18 C19 C20 C21 3.1(12) . . . . ?
C18 C19 N5 C24 21.4(16) . . . . ?
C18 C19 N5 C22 -144.4(13) . . . . ?
C18 C19 N4 C24 -43.8(14) . . . . ?
C18 C19 N4 C26 169.1(9) . . . . ?
C19 N5 C24 C25 -101.5(11) . . . . ?
C19 N5 C22 C23 74.6(19) . . . . ?
C20 C19 N5 C24 -171.3(9) . . . . ?
C20 C19 N5 C22 23.0(18) . . . . ?
C20 C19 N4 C24 156.9(9) . . . . ?
C20 C19 N4 C26 9.9(16) . . . . ?
C1 N1 C5 C4 11.5(10) . . . . ?
N5 C19 C20 C21 -165.4(9) . . . . ?
C24 N5 C22 C23 -89.7(17) . . . . ?
C25 C24 N4 C19 -47.4(15) . . . . ?
C25 C24 N4 C26 102.3(11) . . . . ?
C27 C26 N4 C19 74.5(15) . . . . ?
C27 C26 N4 C24 -75.9(13) . . . . ?
N4 C19 C20 C21 162.1(9) . . . . ?
C22 N5 C24 C25 64.4(15) . . . . ?
C30 N1 C5 C4 -18.5(10) . . . . ?
C30 C31 C32 C4 7(2) . . . . ?
C32 C31 C30 N1 -9(2) . . . . ?
