# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2026508'
loop_
_audit_author_name
_audit_author_address
'Celia Castillo'
;UAM
Spain
;
_audit_update_record             
;
2020-08-31 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[TPnA][Fe(Dca)3]'
_chemical_name_common            
;
Tetrapentylammonium cobalt(II) dicyanamide
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C20 H44 N1), (Fe1 C6 N9)'
_chemical_formula_sum            'C26 H44 Fe1 N10'
_chemical_formula_weight         552.56

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.1007(6)
_cell_length_b                   11.6128(5)
_cell_length_c                   20.0929(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3056.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2464
_cell_measurement_theta_min      4.0250
_cell_measurement_theta_max      64.1490

_exptl_crystal_description       tetrahedral
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_F_000             1184.7
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    4.200
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85332
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_probe          x-ray
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1183
_diffrn_reflns_number            6312
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.1989
_diffrn_reflns_theta_max         64.3769
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_max 0.9921
_diffrn_measured_fraction_theta_full 0.9351
_diffrn_orient_matrix_UB_11      0.1112732000
_diffrn_orient_matrix_UB_12      -0.0425234000
_diffrn_orient_matrix_UB_13      -0.0035041000
_diffrn_orient_matrix_UB_21      0.0354363000
_diffrn_orient_matrix_UB_22      0.1086637000
_diffrn_orient_matrix_UB_23      0.0374462000
_diffrn_orient_matrix_UB_31      -0.0139700000
_diffrn_orient_matrix_UB_32      -0.0630051000
_diffrn_orient_matrix_UB_33      0.0668334000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -53.00   17.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      -51.2500   30.0000  -90.0000 70

#__ type_ start__ end____ width___ exp.time_
  2 omega  -18.00   12.00   1.0000   16.4900
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega   33.00   80.00   1.0000   16.4900
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 47

#__ type_ start__ end____ width___ exp.time_
  4 omega   67.00  122.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -       51.2500  153.0000 -142.0000 55

#__ type_ start__ end____ width___ exp.time_
  5 omega  121.00  147.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  108.00  134.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega  146.00  172.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
  8 omega  119.00  145.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   64.00  101.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000   43.0000    0.0000 37

#__ type_ start__ end____ width___ exp.time_
 10 omega   37.00   73.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000   30.0000 36

#__ type_ start__ end____ width___ exp.time_
 11 omega   41.00   89.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000    0.0000 48

#__ type_ start__ end____ width___ exp.time_
 12 omega   42.00   67.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   77.00  106.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -153.0000  176.0000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega   24.00   50.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -153.0000  176.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   20.00   70.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000 -104.0000   30.0000 50

#__ type_ start__ end____ width___ exp.time_
 16 omega   25.00   59.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  -30.0000 34

#__ type_ start__ end____ width___ exp.time_
 17 omega   33.00   88.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000  -90.0000 55

#__ type_ start__ end____ width___ exp.time_
 18 omega   25.00   66.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000 -150.0000 41

#__ type_ start__ end____ width___ exp.time_
 19 omega   22.00   68.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000  150.0000 46

#__ type_ start__ end____ width___ exp.time_
 20 omega   43.00   71.00   1.0000   16.4900
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
 21 omega -132.00  -25.00   1.0000   65.9600
omega____ theta____ kappa____ phi______ frames
    -      -51.2500  -77.0000  150.0000 107

;
_symmetry_space_group_name_H-M_alt 'P n n a'
_symmetry_space_group_name_H-M   'P n n a'
_symmetry_cell_setting           orthorhombic
_reflns_odcompleteness_completeness 93.51
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1

_reflns_number_total             2546
_reflns_number_gt                2066
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0609P)²+0.7873P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2546
_refine_ls_number_parameters     207
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1090
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Fe1 Fe 0.250000 0.500000 0.09708(2) 0.04651(18) Uani 1 2 d S T P . .
N3 N 0.19228(17) 0.3847(2) 0.17230(11) 0.0682(6) Uani 1 1 d . . . . .
N2 N 0.17196(17) 0.39992(19) 0.02209(11) 0.0677(6) Uani 1 1 d . . . . .
C1 C -0.0333(2) 0.3647(2) -0.07559(13) 0.0614(6) Uani 1 1 d . . . . .
N1' N 0.0622(15) 0.335(4) -0.0696(14) 0.089(6) Uani 0.55(7) 1 d . . P . .
N1 N 0.0441(19) 0.3084(10) -0.0465(19) 0.069(6) Uani 0.45(7) 1 d . . P . .
N4 N -0.11133(17) 0.39416(19) -0.09345(10) 0.0629(6) Uani 1 1 d . . . . .
C2 C 0.1138(2) 0.3687(2) -0.01546(14) 0.0647(7) Uani 1 1 d . . . . .
C3 C 0.16404(18) 0.3192(2) 0.20972(12) 0.0580(6) Uani 1 1 d . . . . .
N5 N 0.1193(3) 0.250000 0.250000 0.1132(16) Uani 1 2 d S T P . .
N6 N 0.250000 0.000000 0.06720(17) 0.0644(8) Uani 0.414(9) 2 d S T P A 1
C4 C 0.3993(4) 0.3510(4) -0.1548(2) 0.1341(17) Uani 0.414(9) 1 d . . P A 1
H4A H 0.454439 0.359214 -0.185905 0.201 Uiso 0.414(9) 1 calc R U P A 1
H4B H 0.335785 0.347361 -0.178467 0.201 Uiso 0.414(9) 1 calc R U P A 1
H4C H 0.398621 0.415775 -0.125125 0.201 Uiso 0.414(9) 1 calc R U P A 1
C5 C 0.4138(3) 0.2414(4) -0.1151(2) 0.1125(13) Uani 0.414(9) 1 d . . P A 1
H5A H 0.415983 0.176412 -0.145387 0.135 Uiso 0.414(9) 1 calc R U P A 1
H5B H 0.478815 0.244820 -0.092049 0.135 Uiso 0.414(9) 1 calc R U P A 1
C6 C 0.3326(3) 0.2226(3) -0.06635(16) 0.0855(9) Uani 0.414(9) 1 d . . P A 1
H6A H 0.268087 0.217858 -0.089899 0.103 Uiso 0.414(9) 1 calc R U P A 1
H6B H 0.329319 0.289216 -0.037316 0.103 Uiso 0.414(9) 1 calc R U P A 1
C7 C 0.3440(3) 0.1151(3) -0.02328(17) 0.0926(10) Uani 0.414(9) 1 d . . P A 1
H7A H 0.345063 0.047031 -0.051271 0.111 Uiso 0.414(9) 1 calc R U P A 1
H7B H 0.407848 0.118371 0.001122 0.111 Uiso 0.414(9) 1 calc R U P A 1
C8 C 0.2560(2) 0.1082(2) 0.02471(15) 0.0721(8) Uani 0.414(9) 1 d . . P A 1
H8A H 0.193079 0.114589 -0.000479 0.086 Uiso 0.414(9) 1 calc R U P A 1
H8B H 0.259507 0.174196 0.054193 0.086 Uiso 0.414(9) 1 calc R U P A 1
C9 C 0.1549(2) 0.0133(2) 0.11001(15) 0.0714(8) Uani 0.414(9) 1 d . . P A 1
H9A H 0.158565 0.087025 0.132541 0.086 Uiso 0.414(9) 1 calc R U P A 1
H9B H 0.095953 0.015418 0.080838 0.086 Uiso 0.414(9) 1 calc R U P A 1
C10 C 0.1373(3) -0.0792(3) 0.16186(18) 0.0916(10) Uani 0.414(9) 1 d D . P A 1
H10A H 0.178727 -0.067237 0.201279 0.110 Uiso 0.414(9) 1 calc R U P A 1
H10B H 0.149545 -0.155809 0.144285 0.110 Uiso 0.414(9) 1 calc R U P A 1
C11 C 0.0187(8) -0.0566(10) 0.1759(6) 0.083(3) Uani 0.414(9) 1 d D . P A 1
H11A H 0.008298 0.022504 0.189837 0.099 Uiso 0.414(9) 1 calc R U P A 1
H11B H -0.020643 -0.069912 0.135770 0.099 Uiso 0.414(9) 1 calc R U P A 1
C12 C -0.0149(7) -0.1365(8) 0.2292(5) 0.100(4) Uani 0.414(9) 1 d D . P A 1
H12A H 0.027497 -0.124798 0.268200 0.120 Uiso 0.414(9) 1 calc R U P A 1
H12B H -0.004873 -0.215138 0.214253 0.120 Uiso 0.414(9) 1 calc R U P A 1
C13 C -0.1272(11) -0.1205(13) 0.2489(9) 0.116(5) Uani 0.414(9) 1 d D . P A 1
H13A H -0.144551 -0.174232 0.283369 0.175 Uiso 0.414(9) 1 calc R U P A 1
H13B H -0.137495 -0.043373 0.264764 0.175 Uiso 0.414(9) 1 calc R U P A 1
H13C H -0.169879 -0.133753 0.210793 0.175 Uiso 0.414(9) 1 calc R U P A 1
N6' N 0.250000 0.000000 0.06720(17) 0.0644(8) Uani 0.586(9) 2 d S T P A 2
C4' C 0.3993(4) 0.3510(4) -0.1548(2) 0.1341(17) Uani 0.586(9) 1 d . . P A 2
H4D H 0.454439 0.359214 -0.185905 0.201 Uiso 0.586(9) 1 calc R U P A 2
H4E H 0.335785 0.347361 -0.178467 0.201 Uiso 0.586(9) 1 calc R U P A 2
H4F H 0.398621 0.415775 -0.125125 0.201 Uiso 0.586(9) 1 calc R U P A 2
C5' C 0.4138(3) 0.2414(4) -0.1151(2) 0.1125(13) Uani 0.586(9) 1 d . . P A 2
H5C H 0.415983 0.176412 -0.145387 0.135 Uiso 0.586(9) 1 calc R U P A 2
H5D H 0.478815 0.244820 -0.092049 0.135 Uiso 0.586(9) 1 calc R U P A 2
C6' C 0.3326(3) 0.2226(3) -0.06635(16) 0.0855(9) Uani 0.586(9) 1 d . . P A 2
H6C H 0.268087 0.217858 -0.089899 0.103 Uiso 0.586(9) 1 calc R U P A 2
H6D H 0.329319 0.289216 -0.037316 0.103 Uiso 0.586(9) 1 calc R U P A 2
C7' C 0.3440(3) 0.1151(3) -0.02328(17) 0.0926(10) Uani 0.586(9) 1 d . . P A 2
H7C H 0.345063 0.047031 -0.051271 0.111 Uiso 0.586(9) 1 calc R U P A 2
H7D H 0.407848 0.118371 0.001122 0.111 Uiso 0.586(9) 1 calc R U P A 2
C8' C 0.2560(2) 0.1082(2) 0.02471(15) 0.0721(8) Uani 0.586(9) 1 d . . P A 2
H8C H 0.193079 0.114589 -0.000479 0.086 Uiso 0.586(9) 1 calc R U P A 2
H8D H 0.259507 0.174196 0.054193 0.086 Uiso 0.586(9) 1 calc R U P A 2
C9' C 0.1549(2) 0.0133(2) 0.11001(15) 0.0714(8) Uani 0.586(9) 1 d . . P A 2
H9C H 0.158565 0.087025 0.132541 0.086 Uiso 0.586(9) 1 calc R U P A 2
H9D H 0.095953 0.015418 0.080838 0.086 Uiso 0.586(9) 1 calc R U P A 2
C10' C 0.1373(3) -0.0792(3) 0.16186(18) 0.0916(10) Uani 0.586(9) 1 d D . P A 2
H10C H 0.198488 -0.085985 0.188791 0.110 Uiso 0.586(9) 1 calc R U P A 2
H10D H 0.127655 -0.152141 0.139152 0.110 Uiso 0.586(9) 1 calc R U P A 2
C11' C 0.0467(5) -0.0596(6) 0.2081(3) 0.075(2) Uani 0.586(9) 1 d D . P A 2
H11C H 0.056417 -0.101818 0.249262 0.090 Uiso 0.586(9) 1 calc R U P A 2
H11D H 0.040830 0.021642 0.218730 0.090 Uiso 0.586(9) 1 calc R U P A 2
C12' C -0.0477(5) -0.0998(6) 0.1742(3) 0.087(2) Uani 0.586(9) 1 d D . P A 2
H12C H -0.042793 -0.182020 0.166209 0.104 Uiso 0.586(9) 1 calc R U P A 2
H12D H -0.053745 -0.061704 0.131436 0.104 Uiso 0.586(9) 1 calc R U P A 2
C13' C -0.1416(8) -0.0755(11) 0.2149(6) 0.129(4) Uani 0.586(9) 1 d D . P A 2
H13D H -0.200764 -0.102631 0.191466 0.194 Uiso 0.586(9) 1 calc R U P A 2
H13E H -0.136447 -0.114340 0.256910 0.194 Uiso 0.586(9) 1 calc R U P A 2
H13F H -0.147390 0.005894 0.222160 0.194 Uiso 0.586(9) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Fe1 N3 2.156(2) . ?
Fe1 N3 2.156(2) 2_565 ?
Fe1 N2 2.160(2) 2_565 ?
Fe1 N2 2.160(2) . ?
Fe1 N4 2.195(2) 6_655 ?
Fe1 N4 2.195(2) 5_565 ?
N3 C3 1.132(3) . ?
N2 C2 1.132(3) . ?
C1 N4 1.136(3) . ?
C1 N1' 1.302(14) . ?
C1 N1 1.341(16) . ?
N1' N1 0.608(19) . ?
N1' C2 1.339(13) . ?
N1 C2 1.309(16) . ?
C3 N5 1.282(3) . ?
N6 C8 1.521(3) . ?
N6 C8 1.521(3) 2 ?
N6 C9 1.522(4) 2 ?
N6 C9 1.522(4) . ?
C4 C5 1.514(5) . ?
C5 C6 1.462(5) . ?
C6 C7 1.527(4) . ?
C7 C8 1.505(4) . ?
C9 C10 1.514(4) . ?
C10 C11 1.601(11) . ?
C11 C12 1.484(15) . ?
C12 C13 1.535(15) . ?
N6' C8' 1.521(3) . ?
N6' C9' 1.522(4) . ?
C4' C5' 1.514(5) . ?
C5' C6' 1.462(5) . ?
C6' C7' 1.527(4) . ?
C7' C8' 1.505(4) . ?
C9' C10' 1.514(4) . ?
C10' C11' 1.525(7) . ?
C11' C12' 1.487(10) . ?
C12' C13' 1.502(11) . ?

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
N3 Fe1 N3 90.99(13) . 2_565 ?
N3 Fe1 N2 171.51(8) . 2_565 ?
N3 Fe1 N2 89.36(9) 2_565 2_565 ?
N3 Fe1 N2 89.36(9) . . ?
N3 Fe1 N2 171.51(8) 2_565 . ?
N2 Fe1 N2 91.54(13) 2_565 . ?
N3 Fe1 N4 88.04(8) . 6_655 ?
N3 Fe1 N4 94.63(8) 2_565 6_655 ?
N2 Fe1 N4 83.47(8) 2_565 6_655 ?
N2 Fe1 N4 93.86(8) . 6_655 ?
N3 Fe1 N4 94.63(8) . 5_565 ?
N3 Fe1 N4 88.04(8) 2_565 5_565 ?
N2 Fe1 N4 93.86(8) 2_565 5_565 ?
N2 Fe1 N4 83.47(8) . 5_565 ?
N4 Fe1 N4 176.19(11) 6_655 5_565 ?
C3 N3 Fe1 176.2(2) . . ?
C2 N2 Fe1 162.9(2) . . ?
N4 C1 N1' 166.5(16) . . ?
N4 C1 N1 164.7(13) . . ?
N1' C1 N1 26.5(8) . . ?
N1 N1' C1 80(3) . . ?
N1 N1' C2 74(3) . . ?
C1 N1' C2 118.9(9) . . ?
N1' N1 C2 79(3) . . ?
N1' N1 C1 73(3) . . ?
C2 N1 C1 118.3(9) . . ?
C1 N4 Fe1 157.5(2) . 5_565 ?
N2 C2 N1 163.4(13) . . ?
N2 C2 N1' 167.1(14) . . ?
N1 C2 N1' 26.5(8) . . ?
N3 C3 N5 171.9(3) . . ?
C3 N5 C3 125.6(4) 4 . ?
C8 N6 C8 111.7(3) . 2 ?
C8 N6 C9 111.03(16) . 2 ?
C8 N6 C9 106.01(14) 2 2 ?
C8 N6 C9 106.02(14) . . ?
C8 N6 C9 111.03(16) 2 . ?
C9 N6 C9 111.1(3) 2 . ?
C6 C5 C4 112.8(3) . . ?
C5 C6 C7 115.5(3) . . ?
C8 C7 C6 109.4(3) . . ?
C7 C8 N6 116.3(2) . . ?
C10 C9 N6 116.2(2) . . ?
C9 C10 C11 98.8(5) . . ?
C12 C11 C10 108.2(7) . . ?
C11 C12 C13 113.2(9) . . ?
C8' N6' C9' 106.02(14) . . ?
C6' C5' C4' 112.8(3) . . ?
C5' C6' C7' 115.5(3) . . ?
C8' C7' C6' 109.4(3) . . ?
C7' C8' N6' 116.3(2) . . ?
C10' C9' N6' 116.2(2) . . ?
C9' C10' C11' 115.6(4) . . ?
C12' C11' C10' 108.8(5) . . ?
C11' C12' C13' 111.9(6) . . ?

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.040



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2026496'
loop_
_audit_author_name
_audit_author_address
'Celia Castillo Blas'
;UAM
Spain
;
_audit_update_record             
;
2020-08-31 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[TPnA][Co(Dca)3]'
_chemical_name_common            
;
Tetrapentylammonium cobalt(II) dicyanamide
;
_chemical_melting_point          ?
_chemical_formula_moiety         '(C20 H44 N1), (Co1 C6 N9)'
_chemical_formula_sum            'C26 H44 Co1 N10'
_chemical_formula_weight         555.73

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.066(2)
_cell_length_b                   11.6026(19)
_cell_length_c                   19.926(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3020.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1573
_cell_measurement_theta_min      3.8980
_cell_measurement_theta_max      63.5190

_exptl_crystal_description       tetrahedral
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_F_000             1336.00
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    4.69897
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_probe          x-ray
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1183
_diffrn_reflns_number            2570
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.2173
_diffrn_reflns_theta_max         64.1699
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measured_fraction_theta_full 0.9333
_diffrn_orient_matrix_UB_11      -0.1038941000
_diffrn_orient_matrix_UB_12      -0.0061930000
_diffrn_orient_matrix_UB_13      -0.0366279000
_diffrn_orient_matrix_UB_21      0.0367143000
_diffrn_orient_matrix_UB_22      0.0920317000
_diffrn_orient_matrix_UB_23      -0.0501036000
_diffrn_orient_matrix_UB_31      0.0424803000
_diffrn_orient_matrix_UB_32      -0.0954148000
_diffrn_orient_matrix_UB_33      -0.0459703000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   70.00   96.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500 -125.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega   89.00  126.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -89.0000  -60.0000 37

#__ type_ start__ end____ width___ exp.time_
  3 omega   40.00   74.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega   29.00   74.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  5 omega   32.00   73.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -43.0000 -150.0000 41

#__ type_ start__ end____ width___ exp.time_
  6 omega   32.00   59.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -89.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega   28.00   85.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000   60.0000 57

#__ type_ start__ end____ width___ exp.time_
  8 omega   40.00   69.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -32.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
  9 omega   36.00  128.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -11.0000  120.0000 92

#__ type_ start__ end____ width___ exp.time_
 10 omega  150.00  175.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   82.00  113.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  104.0000   90.0000 31

#__ type_ start__ end____ width___ exp.time_
 12 omega   74.00  131.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000    0.0000 57

#__ type_ start__ end____ width___ exp.time_
 13 omega   48.00   83.00   1.0000   13.0300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 35

#__ type_ start__ end____ width___ exp.time_
 14 omega   35.00   60.00   1.0000   13.0300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 15 omega   -3.00   52.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500 -125.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
 16 omega   32.00   78.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      102.5000  -54.0000  150.0000 46

#__ type_ start__ end____ width___ exp.time_
 17 omega   38.00   85.00   1.0000   13.0300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  120.0000 47

#__ type_ start__ end____ width___ exp.time_
 18 omega   73.00  114.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -       51.2500  125.0000 -180.0000 41

#__ type_ start__ end____ width___ exp.time_
 19 omega -124.00  -44.00   1.0000   52.1250
omega____ theta____ kappa____ phi______ frames
    -      -51.2500  -61.0000    0.0000 80

;

_symmetry_space_group_name_H-M_alt 'P n n a'
_symmetry_space_group_name_H-M   'P n n a'
_symmetry_cell_setting           orthorhombic
_reflns_odcompleteness_completeness 93.33
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1

_reflns_number_total             2520
_reflns_number_gt                1720
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0989P)²+2.9499P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2520
_refine_ls_number_parameters     187
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.2124
_refine_ls_wR_factor_gt          0.1857
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.250000 0.000000 0.40276(4) 0.0467(4) Uani 1 2 d S T P . .
N2 N 0.1124(3) 0.1027(4) 0.40642(19) 0.0613(11) Uani 1 1 d . . . . .
N1 N 0.3262(3) 0.0995(4) 0.4773(2) 0.0657(11) Uani 1 1 d . . . . .
N3 N 0.3069(3) 0.1133(4) 0.3278(2) 0.0657(11) Uani 1 1 d . . . . .
C2 C 0.3862(4) 0.1302(4) 0.5153(3) 0.0630(13) Uani 1 1 d . . . . .
C3 C 0.3342(4) 0.1800(4) 0.2906(2) 0.0570(12) Uani 1 1 d . . . . .
N5 N 0.3780(6) 0.250000 0.250000 0.111(3) Uani 1 2 d S T P . .
C1 C 0.0343(4) 0.1323(4) 0.4242(3) 0.0616(13) Uani 1 1 d . . . . .
N4 N 0.4466(4) 0.1774(5) 0.5589(3) 0.111(2) Uani 1 1 d . . . . .
N6 N 1.250000 0.000000 0.0667(3) 0.0645(16) Uani 1 2 d S T P . .
C6 C 1.1665(5) 0.2227(5) -0.0672(3) 0.0845(17) Uani 1 1 d . . . . .
H6A H 1.169877 0.289214 -0.037797 0.101 Uiso 1 1 calc R U . . .
H6B H 1.230981 0.218561 -0.091289 0.101 Uiso 1 1 calc R U . . .
C8 C 1.2447(5) 0.1086(5) 0.0243(3) 0.0716(15) Uani 1 1 d . . . . .
H8A H 1.241099 0.174502 0.054176 0.086 Uiso 1 1 calc R U . . .
H8B H 1.307887 0.115059 -0.000983 0.086 Uiso 1 1 calc R U . . .
C7 C 1.1563(6) 0.1154(5) -0.0242(3) 0.095(2) Uani 1 1 d . . . . .
H7A H 1.092251 0.117918 0.000390 0.114 Uiso 1 1 calc R U . . .
H7B H 1.155654 0.047533 -0.052638 0.114 Uiso 1 1 calc R U . . .
C5 C 1.0843(6) 0.2418(7) -0.1162(4) 0.109(2) Uani 1 1 d . . . . .
H5A H 1.019251 0.245824 -0.092820 0.130 Uiso 1 1 calc R U . . .
H5B H 1.081556 0.177075 -0.146928 0.130 Uiso 1 1 calc R U . . .
C4 C 1.1004(7) 0.3518(7) -0.1556(4) 0.134(3) Uani 1 1 d . . . . .
H4A H 1.049199 0.357686 -0.189990 0.200 Uiso 1 1 calc R U . . .
H4B H 1.167063 0.350778 -0.175836 0.200 Uiso 1 1 calc R U . . .
H4C H 1.095123 0.416819 -0.125980 0.200 Uiso 1 1 calc R U . . .
C9 C 1.1543(5) -0.0132(4) 0.1100(3) 0.0715(15) Uani 0.607(13) 1 d . . P A 1
H9A H 1.154525 -0.089553 0.129836 0.086 Uiso 0.607(13) 1 calc R U P A 1
H9B H 1.094557 -0.007978 0.081174 0.086 Uiso 0.607(13) 1 calc R U P A 1
C10 C 1.1436(14) 0.0799(16) 0.1686(9) 0.072(4) Uani 0.607(13) 1 d . . P A 1
H10A H 1.202783 0.075658 0.197808 0.086 Uiso 0.607(13) 1 calc R U P A 1
H10B H 1.141042 0.156649 0.149322 0.086 Uiso 0.607(13) 1 calc R U P A 1
C11 C 1.0474(7) 0.0580(9) 0.2088(6) 0.077(3) Uani 0.607(13) 1 d D . P A 1
H11A H 1.054082 0.094890 0.252308 0.093 Uiso 0.607(13) 1 calc R U P A 1
H11B H 1.040401 -0.024213 0.216333 0.093 Uiso 0.607(13) 1 calc R U P A 1
C12 C 0.9497(8) 0.1030(11) 0.1743(6) 0.092(4) Uani 0.607(13) 1 d D . P A 1
H12A H 0.923612 0.048414 0.141650 0.110 Uiso 0.607(13) 1 calc R U P A 1
H12B H 0.961181 0.176801 0.152686 0.110 Uiso 0.607(13) 1 calc R U P A 1
C13 C 0.8686(10) 0.1157(13) 0.2430(10) 0.123(5) Uani 0.607(13) 1 d . . P A 1
H13A H 0.803154 0.143692 0.228374 0.184 Uiso 0.607(13) 1 calc R U P A 1
H13B H 0.860332 0.041666 0.263793 0.184 Uiso 0.607(13) 1 calc R U P A 1
H13C H 0.897521 0.168749 0.274718 0.184 Uiso 0.607(13) 1 calc R U P A 1
C9' C 1.1543(5) -0.0132(4) 0.1100(3) 0.0715(15) Uani 0.393(13) 1 d . . P A 2
C10' C 1.127(3) 0.079(3) 0.1506(15) 0.086(11) Uiso 0.393(13) 1 d . . P A 2
H10C H 1.131284 0.150060 0.125043 0.104 Uiso 0.393(13) 1 calc R U P A 2
H10D H 1.174282 0.084478 0.187964 0.104 Uiso 0.393(13) 1 calc R U P A 2
C13' C 0.8520(16) 0.0670(18) 0.2101(10) 0.090(6) Uiso 0.393(13) 1 d . . P A 2
H13D H 0.801520 0.100069 0.239346 0.135 Uiso 0.393(13) 1 calc R U P A 2
H13E H 0.833127 0.081282 0.164244 0.135 Uiso 0.393(13) 1 calc R U P A 2
H13F H 0.855797 -0.014541 0.217680 0.135 Uiso 0.393(13) 1 calc R U P A 2
C12' C 0.9857(15) 0.1372(16) 0.2283(10) 0.102(7) Uiso 0.393(13) 1 d . . P A 2
H12C H 0.990888 0.218382 0.217278 0.122 Uiso 0.393(13) 1 calc R U P A 2
H12D H 1.014162 0.120008 0.272138 0.122 Uiso 0.393(13) 1 calc R U P A 2
C11' C 1.0144(17) 0.0630(17) 0.1780(10) 0.075(5) Uiso 0.393(13) 1 d . . P A 2
H11C H 0.967184 0.072219 0.140817 0.090 Uiso 0.393(13) 1 calc R U P A 2
H11D H 1.007342 -0.015281 0.194391 0.090 Uiso 0.393(13) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N3 2.124(4) . ?
Co1 N3 2.124(4) 2 ?
Co1 N1 2.129(4) . ?
Co1 N1 2.129(4) 2 ?
Co1 N2 2.158(4) . ?
Co1 N2 2.158(4) 2 ?
N2 C1 1.134(6) . ?
N1 C2 1.146(6) . ?
N3 C3 1.129(6) . ?
C2 N4 1.295(7) . ?
C3 N5 1.281(6) . ?
C1 N4 1.304(7) 6_556 ?
N6 C8 1.519(6) . ?
N6 C8 1.519(6) 2_755 ?
N6 C9 1.526(7) 2_755 ?
N6 C9' 1.526(7) . ?
N6 C9 1.526(7) . ?
C6 C5 1.468(8) . ?
C6 C7 1.517(8) . ?
C8 C7 1.509(8) . ?
C5 C4 1.514(9) . ?
C9 C10 1.597(17) . ?
C10 C11 1.51(2) . ?
C11 C12 1.541(3) . ?
C12 C13 1.74(2) . ?
C9' C10' 1.39(3) . ?
C10' C11' 1.58(4) . ?
C13' C12' 1.96(3) . ?
C12' C11' 1.37(2) . ?

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
N3 Co1 N3 90.7(2) . 2 ?
N3 Co1 N1 89.50(18) . . ?
N3 Co1 N1 171.96(16) 2 . ?
N3 Co1 N1 171.96(16) . 2 ?
N3 Co1 N1 89.50(18) 2 2 ?
N1 Co1 N1 91.5(2) . 2 ?
N3 Co1 N2 88.50(16) . . ?
N3 Co1 N2 94.22(16) 2 . ?
N1 Co1 N2 93.82(16) . . ?
N1 Co1 N2 83.46(16) 2 . ?
N3 Co1 N2 94.22(16) . 2 ?
N3 Co1 N2 88.50(16) 2 2 ?
N1 Co1 N2 83.46(16) . 2 ?
N1 Co1 N2 93.82(16) 2 2 ?
N2 Co1 N2 176.1(2) . 2 ?
C1 N2 Co1 158.1(4) . . ?
C2 N1 Co1 161.6(4) . . ?
C3 N3 Co1 174.9(4) . . ?
N1 C2 N4 172.3(6) . . ?
N3 C3 N5 171.8(6) . . ?
C3 N5 C3 127.0(7) . 3 ?
N2 C1 N4 173.5(6) . 6_556 ?
C2 N4 C1 122.7(5) . 6_656 ?
C8 N6 C8 112.4(6) . 2_755 ?
C8 N6 C9 105.5(3) . 2_755 ?
C8 N6 C9 111.1(3) 2_755 2_755 ?
C8 N6 C9' 111.1(3) . . ?
C8 N6 C9' 105.5(3) 2_755 . ?
C8 N6 C9 111.1(3) . . ?
C8 N6 C9 105.5(3) 2_755 . ?
C9 N6 C9 111.3(6) 2_755 . ?
C5 C6 C7 115.7(6) . . ?
C7 C8 N6 115.8(4) . . ?
C8 C7 C6 109.7(5) . . ?
C6 C5 C4 111.7(6) . . ?
N6 C9 C10 114.6(7) . . ?
C11 C10 C9 110.3(12) . . ?
C10 C11 C12 113.2(11) . . ?
C11 C12 C13 100.5(9) . . ?
C10' C9' N6 117.5(16) . . ?
C9' C10' C11' 110(2) . . ?
C11' C12' C13' 81.3(15) . . ?
C12' C11' C10' 115.7(19) . . ?

_refine_diff_density_max         0.288
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.053



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_celiaco
_database_code_depnum_ccdc_archive 'CCDC 2026497'
loop_
_audit_author_name
_audit_author_address
'Celia Castillo Blas'
;UAM
Spain
;
_audit_update_record             
;
2020-08-31 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_audit_creation_date             2020-08-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.13(C48.01 Co8 N72.01), 0.25(C32 H70.35 N2), 0.25(C31.94 H72.29 N2)'
_chemical_formula_sum            'C21.99 H35.67 Co N10'
_chemical_formula_weight         499.06
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   15.7659(6)
_cell_length_b                   15.7712(5)
_cell_length_c                   21.2815(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5291.6(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6708
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      64.356
_cell_measurement_theta_min      3.488
_shelx_estimated_absorpt_T_max   0.619
_shelx_estimated_absorpt_T_min   0.523
_exptl_absorpt_coefficient_mu    5.311
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1350 before and 0.0892 after correction. The Ratio of minimum to maximum transmission is 0.6571. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2117
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1251
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54532
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.370
_diffrn_reflns_theta_max         65.370
_diffrn_reflns_theta_min         2.076
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Vantec 500'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6063
_reflns_number_total             8979
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_coef       0.00011(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8979
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.1093
_refine_ls_restrained_S_all      1.038
_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)+(0.0005P)²+42.7522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2542
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.91(2)
 0.09(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C5B) \\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
Uanis(C52) = Uanis(C51)
Uanis(C56) = Uanis(C55)
Uanis(C66) = Uanis(C67)
Uiso(C75B) = Uiso(C75A)
Uanis(C5B) = Uanis(C5A)
4. Others
 Sof(C71B)=Sof(H71A)=Sof(H71B)=Sof(H70C)=Sof(H70D)=1-FVAR(1)
 Sof(H70A)=Sof(H70B)=Sof(C71A)=Sof(H71C)=Sof(H71D)=FVAR(1)
 Sof(C75B)=Sof(H75A)=Sof(H75B)=Sof(H74C)=Sof(H74D)=1-FVAR(2)
 Sof(H74A)=Sof(H74B)=Sof(C75A)=Sof(H75C)=Sof(H75D)=FVAR(2)
 Sof(C43B)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(3)
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(3)
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(4)
 Sof(C47A)=Sof(H47A)=Sof(H47B)=FVAR(4)
 Sof(H62A)=Sof(H62B)=Sof(C63B)=Sof(H63C)=Sof(H63D)=1-FVAR(5)
 Sof(H62C)=Sof(H62D)=Sof(C63A)=Sof(H63A)=Sof(H63B)=FVAR(5)
 Sof(C64B)=Sof(H64A)=Sof(H64B)=Sof(H64C)=1-FVAR(6)
 Sof(C64A)=Sof(H64D)=Sof(H64E)=Sof(H64F)=FVAR(6)
 Sof(C48B)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(7)
 Sof(H46A)=Sof(H46B)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(7)
 Sof(C72B)=Sof(H72A)=Sof(H72B)=Sof(H72C)=1-FVAR(8)
 Fixed Sof: C5B(0.67) N15A(0.33333) C42A(0.5) H42A(0.5) H42B(0.5) N10A(0.5)
 H41A(0.5) H41B(0.5) H41C(0.5) H41D(0.5) C76B(0.8) H76A(0.8) H76B(0.8)
 H76C(0.8) C5A(0.33333) N15B(0.67) C42B(0.5) H42C(0.5) H42D(0.5) N10B(0.5)
 H72D(0.63) H72E(0.63) H72F(0.63) C76A(0.2) H76D(0.2) H76E(0.2) H76F(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C42A(H42A,H42B), C65(H65A,H65B), C54(H54A,H54B), C66(H66A,H66B), C67(H67A,
 H67B), C46(H46A,H46B), C62(H62A,H62B), C62(H62C,H62D), C75B(H75A,H75B),
 C61(H61A,H61B), C69(H69A,H69B), C74(H74C,H74D), C74(H74A,H74B), C49(H49A,H49B),
  C55(H55A,H55B), C50(H50A,H50B), C40(H40A,H40B), C73(H73A,H73B), C71B(H71A,
 H71B), C70(H70C,H70D), C70(H70A,H70B), C51(H51A,H51B), C41(H41A,H41B),
 C41(H41C,H41D), C53(H53A,H53B), C63B(H63C,H63D), C45(H45A,H45B), C42B(H42C,
 H42D), C71A(H71C,H71D), C75A(H75C,H75D), C47A(H47A,H47B), C63A(H63A,H63B),
 C5(H5A,H5B)
5.b Idealised Me refined as rotating group:
 C43B(H43A,H43B,H43C), C48B(H48A,H48B,H48C), C64B(H64A,H64B,H64C), C56(H56A,
 H56B,H56C), C52(H52A,H52B,H52C), C68(H68A,H68B,H68C), C76B(H76A,H76B,H76C),
 C72B(H72A,H72B,H72C), C48A(H48D,H48E,H48F), C72A(H72D,H72E,H72F), C43A(H43D,
 H43E,H43F), C64A(H64D,H64E,H64F), C76A(H76D,H76E,H76F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.5000 0.5000 0.17769(11) 0.0331(7) Uani 1 2 d S T P . .
Co2 Co 0.0000 0.0000 0.17755(11) 0.0334(7) Uani 1 2 d S T P . .
Co3 Co 0.0000 0.5000 0.31698(10) 0.0285(7) Uani 1 2 d S T P A .
Co4 Co 0.5000 0.0000 0.32808(11) 0.0291(7) Uani 1 2 d S T P . .
N1 N 0.4874(9) 0.4136(7) 0.1018(5) 0.045(3) Uani 1 1 d . . . . .
N16 N 0.0963(8) 0.5074(10) 0.2519(5) 0.048(3) Uani 1 1 d . . . . .
N4 N 0.4893(10) 0.1338(9) 0.3211(5) 0.058(4) Uani 1 1 d . . . . .
N11 N -0.0901(7) 0.5027(9) 0.3946(5) 0.041(3) Uani 1 1 d . . . . .
N14 N 0.0084(9) 0.3667(7) 0.3159(6) 0.044(3) Uani 1 1 d . . . . .
N6 N 0.1325(7) -0.0136(8) 0.1818(5) 0.043(3) Uani 1 1 d . . . . .
N18 N 0.3613(9) 0.5059(10) 0.1808(5) 0.056(3) Uani 1 1 d . . . . .
N9 N -0.0029(10) 0.0939(7) 0.1044(5) 0.050(3) Uani 1 1 d . . . . .
N8 N 0.3967(7) -0.0109(9) 0.2604(5) 0.047(3) Uani 1 1 d . . . . .
N2 N 0.4964(11) 0.4000(7) 0.2448(5) 0.051(3) Uani 1 1 d . . . . .
N5 N 0.4096(9) -0.0110(9) 0.4012(5) 0.057(4) Uani 1 1 d . . . . .
N12 N 0.0106(9) 0.1003(8) 0.2421(5) 0.049(3) Uani 1 1 d . . . . .
N13 N 0.0245(10) 0.2112(8) 0.3196(7) 0.071(5) Uani 1 1 d . . . . .
N3 N 0.4796(13) 0.2867(9) 0.3225(6) 0.086(6) Uani 1 1 d . . . . .
C2 C 0.4872(12) 0.3451(9) 0.2786(6) 0.050(4) Uani 1 1 d . . . . .
N17 N 0.2116(7) 0.5141(10) 0.1755(5) 0.057(4) Uani 1 1 d . . . . .
C5B C -0.115(3) 0.5253(14) 0.4426(19) 0.030(5) Uani 0.67 1 d . U . A 2
C6 C 0.0194(9) 0.2974(13) 0.3119(7) 0.056(5) Uani 1 1 d . . . . .
C8 C -0.0107(15) 0.1171(8) 0.0541(6) 0.056(5) Uani 1 1 d . . . . .
C4 C 0.1552(9) 0.5100(10) 0.2202(6) 0.041(3) Uani 1 1 d . . . . .
C9 C 0.2049(12) -0.0178(9) 0.1877(7) 0.049(4) Uani 1 1 d . . . . .
C3 C 0.2933(9) 0.5130(10) 0.1827(6) 0.041(3) Uani 1 1 d . . . . .
N7 N 0.2873(10) -0.0328(11) 0.1815(7) 0.076(5) Uani 1 1 d . . . . .
C10 C 0.3419(9) -0.0180(8) 0.2271(6) 0.035(3) Uani 1 1 d . . . . .
C12 C 0.4871(9) 0.2073(8) 0.3167(6) 0.037(3) Uani 1 1 d . . . . .
C7 C 0.0152(8) 0.1586(8) 0.2748(6) 0.036(3) Uani 1 1 d . . . . .
C1 C 0.4820(15) 0.3868(11) 0.0524(8) 0.075(6) Uani 1 1 d . . . . .
N15A N -0.159(2) 0.516(2) 0.4972(17) 0.023(9) Uiso 0.3333 1 d . . . A 1
C43B C 0.330(5) 0.525(4) 0.590(3) 0.14(3) Uiso 0.54(7) 1 d . . . B 2
H43A H 0.3904 0.5218 0.5869 0.205 Uiso 0.54(7) 1 calc GR . . B 2
H43B H 0.3114 0.5818 0.5826 0.205 Uiso 0.54(7) 1 calc GR . . B 2
H43C H 0.3047 0.4878 0.5593 0.205 Uiso 0.54(7) 1 calc GR . . B 2
C42A C 0.348(4) 0.438(4) 0.586(3) 0.13(2) Uiso 0.5 1 d . . . B 1
H42A H 0.2977 0.4414 0.5599 0.152 Uiso 0.5 1 calc R . . B 1
H42B H 0.3909 0.4033 0.5650 0.152 Uiso 0.5 1 calc R . . B 1
N10A N -0.0589(19) 0.1430(17) 0.0056(13) 0.046(7) Uiso 0.5 1 d . . . C 2
C48B C 0.468(4) 0.188(4) 0.498(3) 0.08(2) Uiso 0.42(7) 1 d . . . D 2
H48A H 0.4279 0.1534 0.5204 0.126 Uiso 0.42(7) 1 calc GR . . D 2
H48B H 0.5206 0.1894 0.5211 0.126 Uiso 0.42(7) 1 calc GR . . D 2
H48C H 0.4782 0.1637 0.4573 0.126 Uiso 0.42(7) 1 calc GR . . D 2
N40 N 0.2739(8) 0.2568(8) 0.6308(6) 0.055(4) Uani 1 1 d . . . . .
C65 C 0.2095(12) 0.3035(10) 0.1103(8) 0.061(5) Uani 1 1 d . . . . .
H65A H 0.2314 0.3522 0.1330 0.073 Uiso 1 1 calc R . . . .
H65B H 0.2215 0.3123 0.0660 0.073 Uiso 1 1 calc R . . . .
C54 C 0.7345(18) 0.2393(18) 0.2509(11) 0.109(10) Uani 1 1 d . . . . .
H54A H 0.7216 0.1798 0.2574 0.131 Uiso 1 1 calc R . . . .
H54B H 0.6822 0.2709 0.2561 0.131 Uiso 1 1 calc R . . . .
C66 C 0.1149(14) 0.2998(14) 0.1192(14) 0.111(7) Uani 1 1 d . . . . .
H66A H 0.0943 0.2467 0.1018 0.134 Uiso 1 1 calc R . . . .
H66B H 0.1029 0.2992 0.1639 0.134 Uiso 1 1 calc R . . . .
C67 C 0.0660(15) 0.3711(15) 0.0897(14) 0.111(7) Uani 1 1 d . . . . .
H67A H 0.0757 0.3713 0.0447 0.134 Uiso 1 1 calc R . . . .
H67B H 0.0860 0.4247 0.1064 0.134 Uiso 1 1 calc R . . . .
C46 C 0.3426(14) 0.2379(18) 0.5196(9) 0.103(8) Uani 1 1 d . . . . .
H46A H 0.2917 0.2086 0.5061 0.123 Uiso 0.58(7) 1 calc R . . D 1
H46B H 0.3355 0.2976 0.5101 0.123 Uiso 0.58(7) 1 calc R . . D 1
C64B C 0.248(3) 0.494(3) -0.0031(18) 0.084(15) Uiso 0.57(7) 1 d . . . E 2
H64A H 0.2032 0.4877 0.0269 0.126 Uiso 0.57(7) 1 calc GR . . E 2
H64B H 0.2870 0.4475 0.0008 0.126 Uiso 0.57(7) 1 calc GR . . E 2
H64C H 0.2250 0.4950 -0.0447 0.126 Uiso 0.57(7) 1 calc GR . . E 2
C62 C 0.239(2) 0.1560(16) 0.0220(9) 0.124(10) Uani 1 1 d . . . . .
H62A H 0.2816 0.1988 0.0139 0.148 Uiso 0.51(7) 1 calc R . . F 1
H62B H 0.1860 0.1760 0.0039 0.148 Uiso 0.51(7) 1 calc R . . F 1
H62C H 0.2099 0.2063 0.0068 0.148 Uiso 0.49(7) 1 calc R . . F 2
H62D H 0.2986 0.1615 0.0122 0.148 Uiso 0.49(7) 1 calc R . . F 2
C75B C 0.239(3) 0.204(3) 0.3201(17) 0.063(7) Uiso 0.50(4) 1 d . . . G 2
H75A H 0.1873 0.1699 0.3216 0.076 Uiso 0.50(4) 1 calc R . . G 2
H75B H 0.2878 0.1689 0.3296 0.076 Uiso 0.50(4) 1 calc R . . G 2
C61 C 0.2273(12) 0.1484(10) 0.0920(8) 0.062(5) Uani 1 1 d . . . . .
H61A H 0.2579 0.0986 0.1061 0.075 Uiso 1 1 calc R . . . .
H61B H 0.1676 0.1386 0.1003 0.075 Uiso 1 1 calc R . . . .
C69 C 0.3483(15) 0.2429(13) 0.1212(10) 0.092(8) Uani 1 1 d . . . . .
H69A H 0.3570 0.2520 0.0766 0.111 Uiso 1 1 calc R . . . .
H69B H 0.3631 0.2949 0.1428 0.111 Uiso 1 1 calc R . . . .
C74 C 0.2496(15) 0.2612(14) 0.2489(9) 0.080(7) Uani 1 1 d . . . . .
H74C H 0.2079 0.3064 0.2467 0.097 Uiso 0.50(4) 1 calc R . . G 2
H74D H 0.3058 0.2859 0.2458 0.097 Uiso 0.50(4) 1 calc R . . G 2
H74A H 0.2980 0.2947 0.2357 0.097 Uiso 0.50(4) 1 calc R . . G 1
H74B H 0.2011 0.2990 0.2473 0.097 Uiso 0.50(4) 1 calc R . . G 1
C49 C 0.1942(11) 0.2149(14) 0.6120(13) 0.098(8) Uani 1 1 d . . . . .
H49A H 0.1819 0.2285 0.5685 0.118 Uiso 1 1 calc R . . . .
H49B H 0.1480 0.2365 0.6375 0.118 Uiso 1 1 calc R . . . .
C56 C 0.712(3) 0.2518(18) 0.1342(12) 0.177(13) Uani 1 1 d . . . . .
H56A H 0.6672 0.2110 0.1394 0.266 Uiso 1 1 calc GR . . . .
H56B H 0.7443 0.2381 0.0974 0.266 Uiso 1 1 calc GR . . . .
H56C H 0.6877 0.3073 0.1295 0.266 Uiso 1 1 calc GR . . . .
C55 C 0.764(3) 0.2504(19) 0.1864(12) 0.177(13) Uani 1 1 d . . . . .
H55A H 0.7955 0.3033 0.1858 0.213 Uiso 1 1 calc R . . . .
H55B H 0.8052 0.2057 0.1790 0.213 Uiso 1 1 calc R . . . .
C50 C 0.1996(16) 0.1120(13) 0.6200(13) 0.106(8) Uani 1 1 d . . . . .
H50A H 0.2529 0.0910 0.6034 0.127 Uiso 1 1 calc R . . . .
H50B H 0.1960 0.0966 0.6641 0.127 Uiso 1 1 calc R . . . .
C40 C 0.2597(14) 0.3473(15) 0.6226(11) 0.088(7) Uani 1 1 d . . . . .
H40A H 0.2072 0.3618 0.6438 0.105 Uiso 1 1 calc R . . . .
H40B H 0.2510 0.3578 0.5781 0.105 Uiso 1 1 calc R . . . .
C52 C 0.1264(19) -0.0130(16) 0.5925(14) 0.142(8) Uani 1 1 d . . . . .
H52A H 0.1696 -0.0374 0.5663 0.213 Uiso 1 1 calc GR . . . .
H52B H 0.0725 -0.0377 0.5823 0.213 Uiso 1 1 calc GR . . . .
H52C H 0.1395 -0.0240 0.6358 0.213 Uiso 1 1 calc GR . . . .
N60 N 0.2564(9) 0.2246(8) 0.1323(7) 0.055(4) Uani 1 1 d . . . . .
C73 C 0.2362(13) 0.2013(10) 0.1998(8) 0.068(5) Uani 1 1 d . . . . .
H73A H 0.1770 0.1848 0.2013 0.082 Uiso 1 1 calc R . . . .
H73B H 0.2692 0.1512 0.2100 0.082 Uiso 1 1 calc R . . . .
C71B C 0.471(4) 0.182(4) 0.099(4) 0.08(3) Uiso 0.34(6) 1 d . . . H 2
H71A H 0.4371 0.2053 0.0647 0.097 Uiso 0.34(6) 1 calc R . . H 2
H71B H 0.4976 0.2315 0.1170 0.097 Uiso 0.34(6) 1 calc R . . H 2
C70 C 0.4050(17) 0.176(2) 0.1422(16) 0.159(16) Uani 1 1 d . . . . .
H70C H 0.4249 0.1856 0.1847 0.190 Uiso 0.34(6) 1 calc R . . H 2
H70D H 0.3777 0.1205 0.1403 0.190 Uiso 0.34(6) 1 calc R . . H 2
H70A H 0.3932 0.1263 0.1163 0.190 Uiso 0.66(6) 1 calc R . . H 1
H70B H 0.3880 0.1609 0.1847 0.190 Uiso 0.66(6) 1 calc R . . H 1
C51 C 0.123(2) 0.0732(17) 0.5827(16) 0.142(8) Uani 1 1 d . . . . .
H51A H 0.0699 0.0961 0.5979 0.170 Uiso 1 1 calc R . . . .
H51B H 0.1282 0.0860 0.5383 0.170 Uiso 1 1 calc R . . . .
C41 C 0.331(2) 0.411(2) 0.6466(18) 0.174(17) Uani 1 1 d . . . . .
H41A H 0.3094 0.4557 0.6734 0.209 Uiso 0.5 1 calc R . . B 1
H41B H 0.3788 0.3826 0.6664 0.209 Uiso 0.5 1 calc R . . B 1
H41C H 0.3408 0.4009 0.6910 0.209 Uiso 0.5 1 calc R . . B 2
H41D H 0.3836 0.3985 0.6247 0.209 Uiso 0.5 1 calc R . . B 2
C53 C 0.7974(12) 0.2679(12) 0.3016(7) 0.061(5) Uani 1 1 d . . . . .
H53A H 0.8027 0.3291 0.2995 0.074 Uiso 1 1 calc R . . . .
H53B H 0.8525 0.2440 0.2920 0.074 Uiso 1 1 calc R . . . .
C68 C -0.0290(18) 0.3620(17) 0.1027(15) 0.142(13) Uani 1 1 d . . . . .
H68A H -0.0483 0.3080 0.0876 0.213 Uiso 1 1 calc GR . . . .
H68B H -0.0593 0.4064 0.0814 0.213 Uiso 1 1 calc GR . . . .
H68C H -0.0391 0.3660 0.1471 0.213 Uiso 1 1 calc GR . . . .
C76B C 0.233(2) 0.289(2) 0.3638(17) 0.128(12) Uiso 0.8 1 d . . . G 2
H76A H 0.1756 0.2978 0.3768 0.192 Uiso 0.8 1 calc GR . . G 2
H76B H 0.2523 0.3370 0.3401 0.192 Uiso 0.8 1 calc GR . . G 2
H76C H 0.2685 0.2819 0.4002 0.192 Uiso 0.8 1 calc GR . . G 2
C63B C 0.231(5) 0.562(4) 0.017(3) 0.13(3) Uiso 0.51(7) 1 d . . . E 1
H63C H 0.2220 0.5705 0.0618 0.158 Uiso 0.51(7) 1 calc R . . F 1
H63D H 0.1821 0.5351 -0.0017 0.158 Uiso 0.51(7) 1 calc R . . F 1
C45 C 0.3529(11) 0.2271(14) 0.5907(7) 0.070(5) Uani 1 1 d . . . . .
H45A H 0.4023 0.2590 0.6041 0.084 Uiso 1 1 calc R . . . .
H45B H 0.3637 0.1678 0.5996 0.084 Uiso 1 1 calc R . . . .
C72B C 0.535(4) 0.157(5) 0.064(3) 0.11(3) Uiso 0.42(7) 1 d . . . H 2
H72A H 0.5387 0.1917 0.0273 0.168 Uiso 0.42(7) 1 calc GR . . H 2
H72B H 0.5279 0.0990 0.0527 0.168 Uiso 0.42(7) 1 calc GR . . H 2
H72C H 0.5867 0.1632 0.0883 0.168 Uiso 0.42(7) 1 calc GR . . H 2
C11 C 0.3844(10) -0.0201(10) 0.4511(7) 0.050(4) Uani 1 1 d . . . . .
C5A C -0.114(5) 0.501(4) 0.445(4) 0.030(5) Uani 0.3333 1 d . U . A 1
N15B N -0.1486(14) 0.5498(14) 0.4949(10) 0.051(6) Uani 0.67 1 d . . . A 2
C48A C 0.498(3) 0.249(3) 0.4976(17) 0.095(15) Uiso 0.60(7) 1 d . . . D 1
H48D H 0.5413 0.2220 0.4726 0.143 Uiso 0.60(7) 1 calc GR . . D 1
H48E H 0.5129 0.2443 0.5413 0.143 Uiso 0.60(7) 1 calc GR . . D 1
H48F H 0.4949 0.3080 0.4863 0.143 Uiso 0.60(7) 1 calc GR . . D 1
C42B C 0.310(3) 0.505(3) 0.6372(19) 0.088(11) Uiso 0.5 1 d . . . B 2
H42C H 0.2495 0.5137 0.6422 0.105 Uiso 0.5 1 calc R . . B 2
H42D H 0.3392 0.5387 0.6685 0.105 Uiso 0.5 1 calc R . . B 2
N10B N -0.0263(14) 0.1583(14) 0.0010(10) 0.033(6) Uiso 0.5 1 d . . . C 1
C72A C 0.526(3) 0.092(4) 0.097(3) 0.12(3) Uiso 0.55(9) 1 d . . . H 1
H72D H 0.4984 0.0981 0.0574 0.185 Uiso 0.63 1 calc GR . . H 1
H72E H 0.5016 0.0446 0.1195 0.185 Uiso 0.63 1 calc GR . . H 1
H72F H 0.5854 0.0820 0.0911 0.185 Uiso 0.63 1 calc GR . . H 1
C71A C 0.511(2) 0.188(2) 0.1433(18) 0.088(14) Uiso 0.66(6) 1 d . . . H 1
H71C H 0.5356 0.1845 0.1851 0.106 Uiso 0.66(6) 1 calc R . . H 1
H71D H 0.5304 0.2387 0.1219 0.106 Uiso 0.66(6) 1 calc R . . H 1
C75A C 0.262(3) 0.246(3) 0.3080(18) 0.063(7) Uiso 0.50(4) 1 d . . . G 1
H75C H 0.3162 0.2181 0.3130 0.076 Uiso 0.50(4) 1 calc R . . G 1
H75D H 0.2183 0.2076 0.3227 0.076 Uiso 0.50(4) 1 calc R . . G 1
C43A C 0.390(4) 0.544(3) 0.609(2) 0.073(18) Uiso 0.46(7) 1 d . . . B 1
H43D H 0.4034 0.5764 0.5720 0.110 Uiso 0.46(7) 1 calc GR . . B 1
H43E H 0.4395 0.5375 0.6343 0.110 Uiso 0.46(7) 1 calc GR . . B 1
H43F H 0.3471 0.5740 0.6327 0.110 Uiso 0.46(7) 1 calc GR . . B 1
C47A C 0.434(5) 0.276(5) 0.491(4) 0.12(3) Uiso 0.40(7) 1 d . . . D 2
H47A H 0.4304 0.2960 0.4479 0.140 Uiso 0.40(7) 1 calc R . . D 2
H47B H 0.4611 0.3181 0.5178 0.140 Uiso 0.40(7) 1 calc R . . D 2
C63A C 0.296(3) 0.579(3) 0.010(2) 0.071(17) Uiso 0.49(7) 1 d . . . E 2
H63A H 0.2968 0.5895 0.0547 0.085 Uiso 0.49(7) 1 calc R . . F 2
H63B H 0.3549 0.5724 -0.0035 0.085 Uiso 0.49(7) 1 calc R . . F 2
C64A C 0.308(4) 0.518(4) 0.004(2) 0.09(2) Uiso 0.43(7) 1 d . . . E 1
H64D H 0.3049 0.4933 -0.0370 0.129 Uiso 0.43(7) 1 calc GR . . E 1
H64E H 0.3157 0.4737 0.0348 0.129 Uiso 0.43(7) 1 calc GR . . E 1
H64F H 0.3547 0.5566 0.0062 0.129 Uiso 0.43(7) 1 calc GR . . E 1
C5 C 0.413(3) 0.206(3) 0.4857(18) 0.079(15) Uiso 0.58(7) 1 d . . . D 1
H5A H 0.3998 0.2109 0.4413 0.095 Uiso 0.58(7) 1 calc R . . D 1
H5B H 0.4183 0.1465 0.4953 0.095 Uiso 0.58(7) 1 calc R . . D 1
C76A C 0.261(6) 0.348(5) 0.361(4) 0.05(2) Uiso 0.2 1 d . . . G 1
H76D H 0.3149 0.3752 0.3587 0.080 Uiso 0.2 1 calc GR . . G 1
H76E H 0.2485 0.3322 0.4033 0.080 Uiso 0.2 1 calc GR . . G 1
H76F H 0.2176 0.3860 0.3458 0.080 Uiso 0.2 1 calc GR . . G 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N1 2.123(11) . ?
Co1 N1 2.123(11) 2_665 ?
Co1 N18 2.189(14) 2_665 ?
Co1 N18 2.189(14) . ?
Co1 N2 2.128(11) 2_665 ?
Co1 N2 2.128(11) . ?
Co2 N6 2.102(11) 2 ?
Co2 N6 2.102(11) . ?
Co2 N9 2.148(12) 2 ?
Co2 N9 2.148(12) . ?
Co2 N12 2.102(12) 2 ?
Co2 N12 2.102(12) . ?
Co3 N16 2.059(11) . ?
Co3 N16 2.059(11) 2_565 ?
Co3 N11 2.179(11) 2_565 ?
Co3 N11 2.179(11) . ?
Co3 N14 2.107(11) 2_565 ?
Co3 N14 2.107(11) . ?
Co4 N4 2.122(14) . ?
Co4 N4 2.122(14) 2_655 ?
Co4 N8 2.181(12) . ?
Co4 N8 2.181(12) 2_655 ?
Co4 N5 2.117(12) . ?
Co4 N5 2.118(12) 2_655 ?
N1 C1 1.14(2) . ?
N16 C4 1.149(17) . ?
N4 C12 1.164(17) . ?
N11 C5B 1.15(4) . ?
N11 C5A 1.13(8) . ?
N14 C6 1.11(2) . ?
N6 C9 1.15(2) . ?
N18 C3 1.080(17) . ?
N9 C8 1.138(16) . ?
N8 C10 1.123(16) . ?
N2 C2 1.137(17) . ?
N5 C11 1.142(17) . ?
N12 C7 1.155(16) . ?
N13 C6 1.37(2) . ?
N13 C7 1.273(17) . ?
N3 C2 1.316(19) . ?
N3 C12 1.264(19) . ?
N17 C4 1.303(18) . ?
N17 C3 1.297(19) . ?
C5B N15B 1.29(4) . ?
C8 N10A 1.35(3) . ?
C8 N10B 1.33(3) . ?
C9 N7 1.33(2) . ?
N7 C10 1.318(19) . ?
C1 N10A 1.47(3) 3 ?
C1 N10B 1.35(3) 3 ?
N15A C11 1.29(4) 3_456 ?
N15A C5A 1.34(9) . ?
C43B C42B 1.10(6) . ?
C42A C41 1.39(6) . ?
C42A C43A 1.87(8) . ?
N10A C1 1.47(3) 3_455 ?
C48B C47A 1.51(11) . ?
N40 C49 1.47(2) . ?
N40 C40 1.46(3) . ?
N40 C53 1.536(19) 3_456 ?
N40 C45 1.581(19) . ?
C65 C66 1.51(3) . ?
C65 N60 1.52(2) . ?
C54 C55 1.46(4) . ?
C54 C53 1.53(3) . ?
C66 C67 1.50(3) . ?
C67 C68 1.53(4) . ?
C46 C45 1.53(2) . ?
C46 C47A 1.68(8) . ?
C46 C5 1.41(4) . ?
C64B C63A 1.57(7) . ?
C62 C61 1.51(2) . ?
C62 C63B 1.77(7) 4_545 ?
C62 C63A 1.49(5) 4_545 ?
C75B C74 1.77(5) . ?
C75B C76B 1.64(5) . ?
C61 N60 1.55(2) . ?
C69 N60 1.50(2) . ?
C69 C70 1.46(3) . ?
C74 C73 1.42(2) . ?
C74 C75A 1.29(4) . ?
C49 C50 1.63(3) . ?
C56 C55 1.38(3) . ?
C50 C51 1.57(3) . ?
C40 C41 1.59(4) . ?
C52 C51 1.38(4) . ?
N60 C73 1.52(2) . ?
C71B C70 1.39(7) . ?
C71B C72B 1.31(8) . ?
C70 C71A 1.69(5) . ?
C41 C42B 1.53(5) . ?
C53 N40 1.535(19) 3_556 ?
C63B C62 1.77(7) 4 ?
C63B C64A 1.42(10) . ?
C11 N15A 1.29(4) 3_556 ?
C11 N15B 1.35(2) 3_556 ?
N15B C11 1.35(2) 3_456 ?
C48A C5 1.53(7) . ?
N10B C1 1.35(3) 3_455 ?
C72A C71A 1.82(6) . ?
C75A C76A 1.96(9) . ?
C63A C62 1.49(5) 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
N1 Co1 N1 80.9(6) . 2_665 ?
N1 Co1 N18 95.1(5) . 2_665 ?
N1 Co1 N18 87.5(5) 2_665 2_665 ?
N1 Co1 N18 87.5(5) . . ?
N1 Co1 N18 95.1(5) 2_665 . ?
N1 Co1 N2 171.4(5) . 2_665 ?
N1 Co1 N2 91.9(4) . . ?
N1 Co1 N2 171.4(5) 2_665 . ?
N1 Co1 N2 91.9(4) 2_665 2_665 ?
N18 Co1 N18 176.5(6) . 2_665 ?
N2 Co1 N18 88.6(6) . 2_665 ?
N2 Co1 N18 88.6(6) 2_665 . ?
N2 Co1 N18 89.1(6) 2_665 2_665 ?
N2 Co1 N18 89.1(6) . . ?
N2 Co1 N2 95.7(6) 2_665 . ?
N6 Co2 N6 175.0(6) . 2 ?
N6 Co2 N9 86.6(5) 2 . ?
N6 Co2 N9 97.1(5) . . ?
N6 Co2 N9 97.1(5) 2 2 ?
N6 Co2 N9 86.6(5) . 2 ?
N6 Co2 N12 88.5(5) 2 . ?
N6 Co2 N12 88.2(5) . . ?
N6 Co2 N12 88.5(5) . 2 ?
N9 Co2 N9 87.2(6) 2 . ?
N12 Co2 N6 88.2(5) 2 2 ?
N12 Co2 N9 172.0(5) . 2 ?
N12 Co2 N9 87.5(4) . . ?
N12 Co2 N9 172.0(5) 2 . ?
N12 Co2 N9 87.5(4) 2 2 ?
N12 Co2 N12 98.4(6) 2 . ?
N16 Co3 N16 95.4(6) . 2_565 ?
N16 Co3 N11 171.8(5) 2_565 2_565 ?
N16 Co3 N11 171.8(5) . . ?
N16 Co3 N11 91.7(4) 2_565 . ?
N16 Co3 N11 91.7(4) . 2_565 ?
N16 Co3 N14 90.2(6) 2_565 2_565 ?
N16 Co3 N14 90.2(6) . . ?
N16 Co3 N14 89.0(6) 2_565 . ?
N16 Co3 N14 89.0(6) . 2_565 ?
N11 Co3 N11 81.4(5) . 2_565 ?
N14 Co3 N11 93.9(5) . . ?
N14 Co3 N11 87.0(5) . 2_565 ?
N14 Co3 N11 87.0(5) 2_565 . ?
N14 Co3 N11 93.9(5) 2_565 2_565 ?
N14 Co3 N14 178.8(7) 2_565 . ?
N4 Co4 N4 171.9(6) . 2_655 ?
N4 Co4 N8 86.3(5) 2_655 . ?
N4 Co4 N8 88.4(6) 2_655 2_655 ?
N4 Co4 N8 88.4(6) . . ?
N4 Co4 N8 86.3(5) . 2_655 ?
N8 Co4 N8 97.3(6) . 2_655 ?
N5 Co4 N4 91.4(5) . 2_655 ?
N5 Co4 N4 94.6(5) . . ?
N5 Co4 N4 94.6(5) 2_655 2_655 ?
N5 Co4 N4 91.4(5) 2_655 . ?
N5 Co4 N8 174.0(5) . 2_655 ?
N5 Co4 N8 88.6(5) . . ?
N5 Co4 N8 88.6(5) 2_655 2_655 ?
N5 Co4 N8 174.0(5) 2_655 . ?
N5 Co4 N5 85.4(8) . 2_655 ?
C1 N1 Co1 161.8(12) . . ?
C4 N16 Co3 173.5(11) . . ?
C12 N4 Co4 177.1(15) . . ?
C5B N11 Co3 154(2) . . ?
C5A N11 Co3 158(4) . . ?
C6 N14 Co3 173.4(14) . . ?
C9 N6 Co2 175.5(12) . . ?
C3 N18 Co1 176.4(15) . . ?
C8 N9 Co2 154.8(11) . . ?
C10 N8 Co4 177.5(12) . . ?
C2 N2 Co1 173.7(16) . . ?
C11 N5 Co4 158.0(14) . . ?
C7 N12 Co2 176.0(11) . . ?
C7 N13 C6 123.3(14) . . ?
C12 N3 C2 127.9(14) . . ?
N2 C2 N3 173.9(16) . . ?
C3 N17 C4 126.2(12) . . ?
N11 C5B N15B 175(4) . . ?
N14 C6 N13 167.3(17) . . ?
N9 C8 N10A 152(3) . . ?
N9 C8 N10B 168.2(18) . . ?
N16 C4 N17 169.0(14) . . ?
N6 C9 N7 166.2(16) . . ?
N18 C3 N17 169.7(17) . . ?
C10 N7 C9 122.2(15) . . ?
N8 C10 N7 169.8(16) . . ?
N4 C12 N3 169.1(15) . . ?
N12 C7 N13 167.7(16) . . ?
N1 C1 N10A 158(2) . 3 ?
N1 C1 N10B 169.8(18) . 3 ?
C11 N15A C5A 116(4) 3_456 . ?
C41 C42A C43A 95(4) . . ?
C8 N10A C1 107(2) . 3_455 ?
C49 N40 C53 110.3(16) . 3_456 ?
C49 N40 C45 113.1(14) . . ?
C40 N40 C49 106.0(15) . . ?
C40 N40 C53 113.5(14) . 3_456 ?
C40 N40 C45 110.3(16) . . ?
C53 N40 C45 103.9(11) 3_456 . ?
C66 C65 N60 114.2(15) . . ?
C55 C54 C53 115(2) . . ?
C67 C66 C65 115.2(19) . . ?
C66 C67 C68 111(2) . . ?
C45 C46 C47A 108(3) . . ?
C5 C46 C45 113(2) . . ?
C61 C62 C63B 116(3) . 4_545 ?
C63A C62 C61 110(2) 4_545 . ?
C76B C75B C74 94(3) . . ?
C62 C61 N60 116.9(15) . . ?
C70 C69 N60 113.9(18) . . ?
C73 C74 C75B 106(2) . . ?
C75A C74 C73 128(3) . . ?
N40 C49 C50 111.8(16) . . ?
C56 C55 C54 125(4) . . ?
C51 C50 C49 107(2) . . ?
N40 C40 C41 118.1(18) . . ?
C65 N60 C61 108.7(12) . . ?
C69 N60 C65 105.3(14) . . ?
C69 N60 C61 110.5(14) . . ?
C69 N60 C73 113.6(14) . . ?
C73 N60 C65 112.8(14) . . ?
C73 N60 C61 106.0(11) . . ?
C74 C73 N60 120.2(15) . . ?
C72B C71B C70 158(7) . . ?
C69 C70 C71A 122(2) . . ?
C71B C70 C69 101(3) . . ?
C52 C51 C50 106(3) . . ?
C42A C41 C40 92(4) . . ?
C42B C41 C40 114(3) . . ?
C54 C53 N40 115.4(16) . 3_556 ?
C64A C63B C62 95(5) . 4 ?
C46 C45 N40 114.6(14) . . ?
N5 C11 N15A 165(2) . 3_556 ?
N5 C11 N15B 166.3(19) . 3_556 ?
N11 C5A N15A 163(7) . . ?
C5B N15B C11 118(2) . 3_456 ?
C43B C42B C41 109(5) . . ?
C8 N10B C1 116.2(17) . 3_455 ?
C70 C71A C72A 91(3) . . ?
C74 C75A C76A 114(4) . . ?
C48B C47A C46 86(5) . . ?
C62 C63A C64B 116(3) 4 . ?
C46 C5 C48A 117(3) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91(2)
2 0.09(2)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_celiap21212
_database_code_depnum_ccdc_archive 'CCDC 2026498'
loop_
_audit_author_name
_audit_author_address
'Celia Castillo Blas'
;UAM
Spain
;
_audit_update_record             
;
2020-08-31 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_audit_creation_date             2020-08-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.13(C48 Fe8 N72), 0.25(C32.02 H72.2 N2), 0.5(C16 H35.64 N)'
_chemical_formula_sum            'C22.01 H35.86 Fe N10'
_chemical_formula_weight         496.39
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Fe Fe -1.1336 3.1974 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   15.7971(7)
_cell_length_b                   15.8093(9)
_cell_length_c                   21.4138(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5347.9(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8450
_cell_measurement_temperature    240
_cell_measurement_theta_max      64.632
_cell_measurement_theta_min      3.475
_shelx_estimated_absorpt_T_max   0.764
_shelx_estimated_absorpt_T_min   0.648
_exptl_absorpt_coefficient_mu    4.747
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1429 before and 0.0966 after correction. The Ratio of minimum to maximum transmission is 0.6634. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'yellowish colourless'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2111
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55212
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.338
_diffrn_reflns_theta_max         65.338
_diffrn_reflns_theta_min         2.063
_diffrn_ambient_temperature      240
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Vantec 500'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6196
_reflns_number_total             9065
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         9065
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.1063
_refine_ls_restrained_S_all      1.048
_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)+(0.1523P)²+21.3446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2999
_refine_ls_wR_factor_ref         0.3279
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.93(3)
 0.07(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Rigid bond restraints
 N11
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
4. Uiso/Uaniso restraints and constraints
Uanis(C62B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uiso(C51B) = Uiso(C51A)
Uanis(C54B) = Uanis(C54A)
Uanis(C50A) = Uanis(C62B)
Uanis(C72) = Uanis(C71B)
5. Others
 Sof(C55B)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(1)
 Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=FVAR(1)
 Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(2)
 Sof(H42A)=Sof(H42B)=Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(2)
 Sof(C51B)=Sof(H51A)=Sof(H51B)=1-FVAR(3)
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(H51E)=FVAR(3)
 Fixed Sof: C63B(0.33333) H63A(0.33333) H63B(0.33333) H63C(0.33333) C62A(0.67)
 H62A(0.67) H62B(0.67) H70C(0.7) H70D(0.7) H70A(0.33333) H70B(0.33333)
 H53C(0.5) H53D(0.5) H53A(0.5) H53B(0.5) C50A(0.33333) H50A(0.33333)
 H50B(0.33333) C50B(0.67) H50C(0.67) H50D(0.67) C54B(0.5) H54A(0.5) H54B(0.5)
 H72D(0.67) H72E(0.67) H72F(0.67) H72A(0.33333) H72B(0.33333) H72C(0.33333)
 C71B(0.67) H71A(0.67) H71B(0.67) C54A(0.5) H54C(0.5) H54D(0.5) C62B(0.33333)
 H62C(0.33333) H62D(0.33333) C71A(0.33333) H71C(0.33333) H71D(0.33333)
 C63A(0.67) H63D(0.67) H63E(0.67) H63F(0.67)
6.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C60(H60A,H60B), C66(H66A,H66B), C62A(H62A,H62B), C48(H48A,
 H48B), C70(H70C,H70D), C70(H70A,H70B), C40(H40A,H40B), C42(H42C,H42D),
 C42(H42A,H42B), C69(H69A,H69B), C65(H65A,H65B), C53(H53C,H53D), C53(H53A,H53B),
  C50A(H50A,H50B), C52(H52A,H52B), C45(H45A,H45B), C50B(H50C,H50D), C49(H49A,
 H49B), C44(H44A,H44B), C54B(H54A,H54B), C46(H46A,H46B), C73(H73A,H73B),
 C75(H75A,H75B), C71B(H71A,H71B), C74(H74A,H74B), C67(H67A,H67B), C51B(H51A,
 H51B), C54A(H54C,H54D), C41(H41A,H41B), C62B(H62C,H62D), C71A(H71C,H71D)
6.b Idealised Me refined as rotating group:
 C63B(H63A,H63B,H63C), C55B(H55A,H55B,H55C), C47(H47A,H47B,H47C), C72(H72D,
 H72E,H72F), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C43A(H43A,H43B,H43C),
 C68(H68A,H68B,H68C), C63A(H63D,H63E,H63F), C55A(H55D,H55E,H55F), C43B(H43D,
 H43E,H43F), C51A(H51C,H51D,H51E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Fe1 Fe 0.0000 0.5000 0.68218(10) 0.0322(6) Uani 1 2 d S T P . .
Fe2 Fe 0.5000 1.0000 0.67252(10) 0.0350(6) Uani 1 2 d S T P . .
Fe3 Fe 1.0000 1.0000 0.82237(10) 0.0364(7) Uani 1 2 d S T P . .
Fe4 Fe 0.5000 0.5000 0.82290(10) 0.0353(6) Uani 1 2 d S T P . .
N12 N -0.0010(9) 0.5924(7) 0.6053(5) 0.056(3) Uani 1 1 d . . . . .
N6 N 0.5087(9) 0.8970(7) 0.7405(5) 0.054(3) Uani 1 1 d . . . . .
N16 N 0.4045(6) 0.4992(9) 0.8970(5) 0.057(3) Uani 1 1 d . . . . .
N13 N 0.0099(9) 0.3996(7) 0.7482(5) 0.055(3) Uani 1 1 d . . . . .
N7 N 0.5100(8) 0.9100(8) 0.5978(5) 0.055(3) Uani 1 1 d . . . . .
N8 N 0.6364(8) 1.0090(9) 0.6785(5) 0.062(3) Uani 1 1 d . . . . .
N10 N 0.8975(7) 1.0064(9) 0.7543(5) 0.056(3) Uani 1 1 d . . . . .
N15 N 0.0091(8) 0.1350(9) 0.8202(5) 0.061(3) Uani 1 1 d . . . . .
N1 N 0.1346(6) 0.5115(7) 0.6848(5) 0.050(3) Uani 1 1 d . . . . .
N4 N 0.5139(7) 0.6366(7) 0.8185(5) 0.048(3) Uani 1 1 d . . . . .
N3 N 0.3992(7) 0.5120(9) 0.7580(5) 0.056(3) Uani 1 1 d . . . . .
N18 N 0.4114(6) 0.4884(8) 1.1013(5) 0.049(3) Uani 1 1 d . . . . .
C1 C 0.0182(9) 0.6164(8) 0.5574(7) 0.049(3) Uani 1 1 d . . . . .
C2 C 0.0096(9) 0.3441(8) 0.7819(6) 0.046(3) Uani 1 1 d . . . . .
C12 C 0.8434(8) 1.0122(10) 0.7211(6) 0.053(3) Uani 1 1 d . . . . .
C11 C 0.7090(7) 1.0130(9) 0.6818(5) 0.044(3) Uani 1 1 d . . . . .
N14 N 0.0082(11) 0.2887(9) 0.8271(5) 0.079(4) Uani 1 1 d . . . . .
C4 C 0.2061(10) 0.5201(8) 0.6861(6) 0.050(3) Uani 1 1 d . . . . .
N9 N 0.7866(8) 1.0175(12) 0.6751(6) 0.085(5) Uani 1 1 d . . . . .
C3 C 0.0109(9) 0.2071(9) 0.8190(5) 0.045(3) Uani 1 1 d . . . . .
C8 C 0.5207(8) 0.7079(10) 0.8144(6) 0.051(4) Uani 1 1 d . . . . .
N2 N 0.2905(7) 0.5278(10) 0.6779(6) 0.072(4) Uani 1 1 d . . . . .
C9 C 0.5200(8) 0.8425(9) 0.7737(6) 0.046(3) Uani 1 1 d . . . . .
N5 N 0.5343(10) 0.7876(7) 0.8190(6) 0.069(4) Uani 1 1 d . . . . .
N11 N 0.0396(11) 0.6543(8) 0.5056(6) 0.082(4) Uani 1 1 d . U . A 1
C10 C 0.5219(9) 0.8830(7) 0.5476(6) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.3436(8) 0.5164(9) 0.7232(7) 0.050(3) Uani 1 1 d . . . . .
N60 N 0.2228(8) 0.2568(8) 0.1326(6) 0.057(3) Uani 1 1 d . . . . .
C61 C 0.2637(15) 0.2513(12) 0.2469(10) 0.091(8) Uani 1 1 d . . . . .
H61A H 0.3070 0.2070 0.2451 0.109 Uiso 1 1 calc R . . B 1
H61B H 0.2920 0.3048 0.2370 0.109 Uiso 1 1 calc R . . B 1
C60 C 0.2019(10) 0.2341(12) 0.1964(9) 0.076(5) Uani 1 1 d . . . C 1
H60A H 0.1896 0.1734 0.1970 0.091 Uiso 1 1 calc R . . C 1
H60B H 0.1492 0.2634 0.2072 0.091 Uiso 1 1 calc R . . C 1
C66 C 0.2983(16) 0.1115(14) 0.1176(12) 0.117(9) Uani 1 1 d . . . . .
H66A H 0.3011 0.0983 0.1622 0.141 Uiso 1 1 calc R . . . .
H66B H 0.2442 0.0900 0.1017 0.141 Uiso 1 1 calc R . . . .
N40 N 0.2564(8) 0.2749(8) 0.6310(6) 0.054(3) Uani 1 1 d . . . . .
C63B C 0.274(3) 0.255(3) 0.369(2) 0.055(11) Uiso 0.3333 1 d . . . C 2
H63A H 0.2555 0.2892 0.4039 0.083 Uiso 0.3333 1 calc GR . . C 2
H63B H 0.3212 0.2830 0.3482 0.083 Uiso 0.3333 1 calc GR . . C 2
H63C H 0.2918 0.2000 0.3834 0.083 Uiso 0.3333 1 calc GR . . C 2
C62A C 0.237(2) 0.256(2) 0.3060(15) 0.080(10) Uani 0.67 1 d . . . C 1
H62A H 0.1907 0.2158 0.3120 0.096 Uiso 0.67 1 calc R . . C 1
H62B H 0.2145 0.3131 0.3134 0.096 Uiso 0.67 1 calc R . . C 1
C48 C 0.2275(12) 0.3518(10) 0.5914(6) 0.067(4) Uani 1 1 d . . . . .
H48A H 0.2581 0.4020 0.6059 0.080 Uiso 1 1 calc R . . . .
H48B H 0.1671 0.3615 0.5992 0.080 Uiso 1 1 calc R . . . .
C70 C 0.1537(17) 0.240(2) 0.0235(9) 0.132(10) Uani 1 1 d . . . . .
H70C H 0.2043 0.2123 0.0069 0.158 Uiso 0.7 1 calc R . . D 2
H70D H 0.1572 0.3008 0.0140 0.158 Uiso 0.7 1 calc R . . D 2
H70A H 0.1811 0.1894 0.0068 0.158 Uiso 0.3333 1 calc R . . E 1
H70B H 0.1946 0.2864 0.0183 0.158 Uiso 0.3333 1 calc R . . E 1
C40 C 0.2320(11) 0.2992(10) 0.6980(6) 0.058(4) Uani 1 1 d . . . . .
H40A H 0.2601 0.3525 0.7087 0.070 Uiso 1 1 calc R . . . .
H40B H 0.1708 0.3092 0.6996 0.070 Uiso 1 1 calc R . . . .
C42 C 0.2425(17) 0.267(2) 0.8108(11) 0.155(13) Uani 1 1 d . . . . .
H42C H 0.2781 0.3176 0.8119 0.186 Uiso 0.54(9) 1 calc R . . F 2
H42D H 0.1841 0.2877 0.8106 0.186 Uiso 0.54(9) 1 calc R . . F 2
H42A H 0.1861 0.2918 0.8157 0.186 Uiso 0.46(9) 1 calc R . . F 1
H42B H 0.2853 0.3096 0.8210 0.186 Uiso 0.46(9) 1 calc R . . F 1
C69 C 0.1467(9) 0.2266(13) 0.0911(7) 0.071(5) Uani 1 1 d . . . . .
H69A H 0.1386 0.1659 0.0983 0.085 Uiso 1 1 calc R . . . .
H69B H 0.0955 0.2554 0.1057 0.085 Uiso 1 1 calc R . . . .
C65 C 0.3004(9) 0.2111(13) 0.1091(8) 0.075(5) Uani 1 1 d . . . . .
H65A H 0.3501 0.2333 0.1310 0.090 Uiso 1 1 calc R . . . .
H65B H 0.3075 0.2238 0.0646 0.090 Uiso 1 1 calc R . . . .
C53 C 0.4065(13) 0.3305(16) 0.6458(15) 0.123(9) Uani 1 1 d . . . . .
H53C H 0.3759 0.3800 0.6616 0.148 Uiso 0.5 1 calc R . . G 2
H53D H 0.4474 0.3109 0.6771 0.148 Uiso 0.5 1 calc R . . G 2
H53A H 0.3896 0.3837 0.6259 0.148 Uiso 0.5 1 calc R . . H 1
H53B H 0.4002 0.3377 0.6911 0.148 Uiso 0.5 1 calc R . . H 1
C50A C 0.224(5) 0.411(4) 0.479(3) 0.069(12) Uani 0.3333 1 d . . . I 1
H50A H 0.1641 0.4076 0.4683 0.083 Uiso 0.3333 1 calc R . . I 1
H50B H 0.2557 0.3990 0.4403 0.083 Uiso 0.3333 1 calc R . . I 1
C52 C 0.3472(12) 0.2604(10) 0.6241(9) 0.075(5) Uani 1 1 d . . . . .
H52A H 0.3587 0.2495 0.5798 0.090 Uiso 1 1 calc R . . . .
H52B H 0.3616 0.2088 0.6471 0.090 Uiso 1 1 calc R . . . .
C45 C 0.1164(12) 0.1987(15) 0.6157(11) 0.099(7) Uani 1 1 d . . . . .
H45A H 0.0957 0.2505 0.5956 0.119 Uiso 1 1 calc R . . . .
H45B H 0.1014 0.2022 0.6600 0.119 Uiso 1 1 calc R . . . .
C55B C 0.532(3) 0.335(4) 0.585(2) 0.098(17) Uiso 0.52(6) 1 d . . . J 2
H55A H 0.5597 0.3491 0.6236 0.147 Uiso 0.52(6) 1 calc GR . . J 2
H55B H 0.5521 0.3721 0.5519 0.147 Uiso 0.52(6) 1 calc GR . . J 2
H55C H 0.5450 0.2767 0.5737 0.147 Uiso 0.52(6) 1 calc GR . . J 2
C47 C -0.0113(16) 0.1286(18) 0.5940(14) 0.132(10) Uani 1 1 d . . . . .
H47A H -0.0228 0.1531 0.6347 0.198 Uiso 1 1 calc GR . . . .
H47B H -0.0373 0.0731 0.5915 0.198 Uiso 1 1 calc GR . . . .
H47C H -0.0345 0.1648 0.5617 0.198 Uiso 1 1 calc GR . . . .
C50B C 0.1906(19) 0.433(4) 0.492(2) 0.15(2) Uani 0.67 1 d . . . I 2
H50C H 0.1611 0.4270 0.4516 0.176 Uiso 0.67 1 calc R . . I 2
H50D H 0.1593 0.4665 0.5223 0.176 Uiso 0.67 1 calc R . . I 2
C49 C 0.2411(18) 0.3430(14) 0.5198(9) 0.110(8) Uani 1 1 d . . . . .
H49A H 0.3003 0.3267 0.5134 0.132 Uiso 1 1 calc R . . I 1
H49B H 0.2064 0.2952 0.5058 0.132 Uiso 1 1 calc R . . I 1
C44 C 0.2141(12) 0.1975(11) 0.6106(11) 0.087(6) Uani 1 1 d . . . . .
H44A H 0.2357 0.1502 0.6355 0.104 Uiso 1 1 calc R . . . .
H44B H 0.2295 0.1868 0.5669 0.104 Uiso 1 1 calc R . . . .
C54B C 0.441(3) 0.344(3) 0.592(3) 0.127(16) Uani 0.5 1 d . . . J 2
H54A H 0.4270 0.4022 0.5791 0.152 Uiso 0.5 1 calc R . . J 2
H54B H 0.4144 0.3064 0.5614 0.152 Uiso 0.5 1 calc R . . J 2
C72 C 0.000(2) 0.246(3) 0.0012(11) 0.184(15) Uani 1 1 d . . . . .
H72D H -0.0437 0.2149 0.0231 0.277 Uiso 0.67 1 calc GR . . K 2
H72E H -0.0215 0.2659 -0.0384 0.277 Uiso 0.67 1 calc GR . . K 2
H72F H 0.0179 0.2938 0.0264 0.277 Uiso 0.67 1 calc GR . . K 2
H72A H 0.0008 0.1928 0.0239 0.277 Uiso 0.3333 1 calc GR . . L 1
H72B H -0.0409 0.2429 -0.0323 0.277 Uiso 0.3333 1 calc GR . . L 1
H72C H -0.0148 0.2914 0.0295 0.277 Uiso 0.3333 1 calc GR . . L 1
C76 C 0.385(3) 0.0284(19) -0.080(2) 0.24(2) Uani 1 1 d . . . . .
H76A H 0.3565 0.0322 -0.0401 0.354 Uiso 1 1 calc GR . . . .
H76B H 0.4080 0.0832 -0.0913 0.354 Uiso 1 1 calc GR . . . .
H76C H 0.4299 -0.0129 -0.0779 0.354 Uiso 1 1 calc GR . . . .
C46 C 0.0684(18) 0.1217(14) 0.5865(14) 0.126(10) Uani 1 1 d . . . . .
H46A H 0.0812 0.1184 0.5418 0.151 Uiso 1 1 calc R . . . .
H46B H 0.0881 0.0693 0.6061 0.151 Uiso 1 1 calc R . . . .
C73 C 0.2420(13) 0.3484(12) 0.1227(10) 0.087(6) Uani 1 1 d . . . . .
H73A H 0.2943 0.3621 0.1451 0.105 Uiso 1 1 calc R . . . .
H73B H 0.2526 0.3577 0.0781 0.105 Uiso 1 1 calc R . . . .
C75 C 0.1875(17) 0.498(2) 0.1364(16) 0.177(16) Uani 1 1 d . . . . .
H75A H 0.2453 0.5112 0.1231 0.212 Uiso 1 1 calc R . . . .
H75B H 0.1761 0.5264 0.1761 0.212 Uiso 1 1 calc R . . . .
C71B C 0.064(4) 0.197(4) -0.008(2) 0.184(15) Uani 0.67 1 d . . . M 2
H71A H 0.0716 0.1891 -0.0533 0.221 Uiso 0.67 1 calc R . . M 2
H71B H 0.0529 0.1417 0.0105 0.221 Uiso 0.67 1 calc R . . M 2
C74 C 0.1765(17) 0.4064(16) 0.1428(13) 0.118(9) Uani 1 1 d . . . . .
H74A H 0.1658 0.3950 0.1871 0.142 Uiso 1 1 calc R . . . .
H74B H 0.1247 0.3913 0.1202 0.142 Uiso 1 1 calc R . . . .
C13 C 0.3843(9) 0.4851(14) 1.0518(7) 0.077(6) Uani 1 1 d . . . . .
C14 C 0.3831(8) 0.4848(14) 0.9458(7) 0.070(5) Uani 1 1 d . . . . .
N17 N 0.3483(8) 0.4588(11) 0.9980(5) 0.076(4) Uani 1 1 d . . . . .
C43A C 0.252(2) 0.233(3) 0.869(2) 0.078(16) Uiso 0.54(9) 1 d . . . F 2
H43A H 0.2744 0.1765 0.8657 0.117 Uiso 0.54(9) 1 calc GR . . F 2
H43B H 0.1971 0.2314 0.8896 0.117 Uiso 0.54(9) 1 calc GR . . F 2
H43C H 0.2902 0.2682 0.8932 0.117 Uiso 0.54(9) 1 calc GR . . F 2
C68 C 0.3642(15) -0.0267(17) 0.0998(15) 0.149(13) Uani 1 1 d . . . . .
H68A H 0.4144 -0.0544 0.0837 0.224 Uiso 1 1 calc GR . . . .
H68B H 0.3143 -0.0510 0.0805 0.224 Uiso 1 1 calc GR . . . .
H68C H 0.3613 -0.0346 0.1447 0.224 Uiso 1 1 calc GR . . . .
C67 C 0.3682(15) 0.0671(16) 0.0851(14) 0.121(9) Uani 1 1 d . . . . .
H67A H 0.4227 0.0902 0.0989 0.145 Uiso 1 1 calc R . . . .
H67B H 0.3634 0.0758 0.0400 0.145 Uiso 1 1 calc R . . . .
C51B C 0.285(4) 0.447(4) 0.489(3) 0.103(9) Uiso 0.37(3) 1 d . . . I 2
H51A H 0.3101 0.4869 0.5186 0.124 Uiso 0.37(3) 1 calc R . . I 2
H51B H 0.3119 0.4470 0.4473 0.124 Uiso 0.37(3) 1 calc R . . I 2
C54A C 0.498(3) 0.314(2) 0.631(3) 0.127(16) Uani 0.5 1 d . . . J 1
H54C H 0.5025 0.2698 0.5990 0.152 Uiso 0.5 1 calc R . . J 1
H54D H 0.5273 0.2934 0.6688 0.152 Uiso 0.5 1 calc R . . J 1
C41 C 0.2546(14) 0.2337(15) 0.7471(8) 0.089(8) Uani 1 1 d . . . . .
H41A H 0.2191 0.1835 0.7413 0.107 Uiso 1 1 calc R . . . .
H41B H 0.3138 0.2167 0.7417 0.107 Uiso 1 1 calc R . . . .
C62B C 0.204(4) 0.246(5) 0.324(3) 0.069(12) Uani 0.3333 1 d . U . C 2
H62C H 0.1625 0.2915 0.3281 0.083 Uiso 0.3333 1 calc R . . C 2
H62D H 0.1751 0.1910 0.3293 0.083 Uiso 0.3333 1 calc R . . C 2
C71A C 0.078(4) 0.261(7) -0.023(4) 0.15(4) Uani 0.3333 1 d . . . M 1
H71C H 0.0820 0.3204 -0.0354 0.176 Uiso 0.3333 1 calc R . . M 1
H71D H 0.0853 0.2265 -0.0609 0.176 Uiso 0.3333 1 calc R . . M 1
C63A C 0.315(3) 0.236(3) 0.360(2) 0.125(14) Uiso 0.67 1 d . . . C 1
H63D H 0.3182 0.1754 0.3673 0.188 Uiso 0.67 1 calc GR . . C 1
H63E H 0.3009 0.2643 0.3990 0.188 Uiso 0.67 1 calc GR . . C 1
H63F H 0.3685 0.2565 0.3447 0.188 Uiso 0.67 1 calc GR . . C 1
C55A C 0.541(3) 0.397(3) 0.607(2) 0.091(17) Uiso 0.48(6) 1 d . . . J 1
H55D H 0.5218 0.4098 0.5654 0.137 Uiso 0.48(6) 1 calc GR . . J 1
H55E H 0.6021 0.3904 0.6073 0.137 Uiso 0.48(6) 1 calc GR . . J 1
H55F H 0.5260 0.4438 0.6350 0.137 Uiso 0.48(6) 1 calc GR . . J 1
C43B C 0.253(3) 0.188(5) 0.852(3) 0.09(2) Uiso 0.46(9) 1 d . . . F 1
H43D H 0.3123 0.1755 0.8570 0.135 Uiso 0.46(9) 1 calc GR . . F 1
H43E H 0.2242 0.1407 0.8326 0.135 Uiso 0.46(9) 1 calc GR . . F 1
H43F H 0.2277 0.1990 0.8927 0.135 Uiso 0.46(9) 1 calc GR . . F 1
C51A C 0.243(3) 0.503(2) 0.4960(15) 0.103(9) Uiso 0.63(3) 1 d . . . I 1
H51C H 0.2212 0.5396 0.4635 0.155 Uiso 0.63(3) 1 calc GR . . I 1
H51D H 0.3032 0.5107 0.5003 0.155 Uiso 0.63(3) 1 calc GR . . I 1
H51E H 0.2151 0.5162 0.5353 0.155 Uiso 0.63(3) 1 calc GR . . I 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Fe1 N12 2.201(11) . ?
Fe1 N12 2.201(11) 2_565 ?
Fe1 N13 2.132(11) . ?
Fe1 N13 2.132(11) 2_565 ?
Fe1 N1 2.135(10) . ?
Fe1 N1 2.135(10) 2_565 ?
Fe2 N6 2.188(10) . ?
Fe2 N6 2.188(10) 2_675 ?
Fe2 N7 2.148(11) 2_675 ?
Fe2 N7 2.148(11) . ?
Fe2 N8 2.163(13) . ?
Fe2 N8 2.164(13) 2_675 ?
Fe3 N10 2.181(11) . ?
Fe3 N10 2.181(11) 2_775 ?
Fe3 N15 2.139(14) 2_665 ?
Fe3 N15 2.139(14) 1_665 ?
Fe3 N18 2.160(10) 4_657 ?
Fe3 N18 2.160(10) 3_567 ?
Fe4 N16 2.190(11) 2_665 ?
Fe4 N16 2.190(11) . ?
Fe4 N4 2.172(11) . ?
Fe4 N4 2.172(11) 2_665 ?
Fe4 N3 2.122(12) 2_665 ?
Fe4 N3 2.122(12) . ?
N12 C1 1.134(16) . ?
N6 C9 1.131(16) . ?
N16 C14 1.122(17) . ?
N13 C2 1.136(16) . ?
N7 C10 1.172(16) . ?
N8 C11 1.150(16) . ?
N10 C12 1.115(16) . ?
N15 Fe3 2.139(14) 1_445 ?
N15 C3 1.141(18) . ?
N1 C4 1.137(17) . ?
N4 C8 1.136(18) . ?
N3 C5 1.153(16) . ?
N18 Fe3 2.160(10) 3_467 ?
N18 C13 1.144(17) . ?
C1 N11 1.307(18) . ?
C2 N14 1.303(17) . ?
C12 N9 1.335(17) . ?
C11 N9 1.236(17) . ?
N14 C3 1.30(2) . ?
C4 N2 1.351(19) . ?
C8 N5 1.28(2) . ?
N2 C5 1.296(17) . ?
C9 N5 1.322(18) . ?
N11 C10 1.312(17) 3_466 ?
C10 N11 1.312(17) 3_566 ?
N60 C60 1.45(2) . ?
N60 C69 1.569(19) . ?
N60 C65 1.51(2) . ?
N60 C73 1.49(2) . ?
C61 C60 1.48(2) . ?
C61 C62A 1.33(4) . ?
C61 C62B 1.91(6) . ?
C66 C65 1.58(3) . ?
C66 C67 1.48(3) . ?
N40 C48 1.551(19) . ?
N40 C40 1.535(17) . ?
N40 C52 1.46(2) . ?
N40 C44 1.46(2) . ?
C63B C62B 1.47(8) . ?
C62A C63A 1.72(5) . ?
C48 C49 1.56(2) . ?
C70 C69 1.47(2) . ?
C70 C71B 1.72(7) . ?
C70 C71A 1.59(7) . ?
C40 C41 1.52(2) . ?
C42 C43A 1.36(5) . ?
C42 C41 1.47(3) . ?
C42 C43B 1.53(6) . ?
C53 C52 1.53(3) . ?
C53 C54B 1.31(5) . ?
C53 C54A 1.51(5) . ?
C50A C49 1.41(6) . ?
C50A C51A 1.53(8) . ?
C45 C44 1.55(3) . ?
C45 C46 1.57(3) . ?
C55B C54B 1.45(6) . ?
C47 C46 1.27(3) . ?
C50B C49 1.74(6) . ?
C50B C51B 1.51(7) . ?
C49 C51B 1.91(7) . ?
C72 C71B 1.28(5) . ?
C72 C71A 1.36(6) . ?
C76 C75 1.73(4) 4_545 ?
C73 C74 1.45(3) . ?
C75 C76 1.73(4) 4 ?
C75 C74 1.46(4) . ?
C13 N17 1.35(2) . ?
C14 N17 1.31(2) . ?
C68 C67 1.52(4) . ?
C54A C55A 1.57(6) . ?

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
N12 Fe1 N12 83.2(6) . 2_565 ?
N13 Fe1 N12 172.3(5) 2_565 2_565 ?
N13 Fe1 N12 90.1(4) 2_565 . ?
N13 Fe1 N12 172.3(5) . . ?
N13 Fe1 N12 90.1(4) . 2_565 ?
N13 Fe1 N13 96.8(6) 2_565 . ?
N13 Fe1 N1 88.5(5) . . ?
N13 Fe1 N1 89.6(5) . 2_565 ?
N13 Fe1 N1 89.6(5) 2_565 . ?
N13 Fe1 N1 88.5(5) 2_565 2_565 ?
N1 Fe1 N12 93.9(5) . 2_565 ?
N1 Fe1 N12 88.3(5) . . ?
N1 Fe1 N12 88.3(5) 2_565 2_565 ?
N1 Fe1 N12 93.9(5) 2_565 . ?
N1 Fe1 N1 177.0(6) . 2_565 ?
N6 Fe2 N6 96.6(6) . 2_675 ?
N7 Fe2 N6 89.9(4) 2_675 2_675 ?
N7 Fe2 N6 173.4(4) 2_675 . ?
N7 Fe2 N6 89.9(4) . . ?
N7 Fe2 N6 173.4(4) . 2_675 ?
N7 Fe2 N7 83.6(6) . 2_675 ?
N7 Fe2 N8 94.2(5) 2_675 . ?
N7 Fe2 N8 94.2(5) . 2_675 ?
N7 Fe2 N8 90.9(5) . . ?
N7 Fe2 N8 90.9(5) 2_675 2_675 ?
N8 Fe2 N6 88.5(5) . 2_675 ?
N8 Fe2 N6 87.0(5) . . ?
N8 Fe2 N6 87.0(5) 2_675 2_675 ?
N8 Fe2 N6 88.5(5) 2_675 . ?
N8 Fe2 N8 173.2(6) . 2_675 ?
N10 Fe3 N10 96.1(6) 2_775 . ?
N15 Fe3 N10 89.0(5) 1_665 2_775 ?
N15 Fe3 N10 89.4(5) 1_665 . ?
N15 Fe3 N10 89.4(5) 2_665 2_775 ?
N15 Fe3 N10 89.0(5) 2_665 . ?
N15 Fe3 N15 177.6(6) 2_665 1_665 ?
N15 Fe3 N18 93.3(5) 1_665 4_657 ?
N15 Fe3 N18 88.6(5) 1_665 3_567 ?
N15 Fe3 N18 88.6(5) 2_665 4_657 ?
N15 Fe3 N18 93.3(5) 2_665 3_567 ?
N18 Fe3 N10 172.3(4) 4_657 . ?
N18 Fe3 N10 91.2(4) 4_657 2_775 ?
N18 Fe3 N10 91.2(4) 3_567 . ?
N18 Fe3 N10 172.2(4) 3_567 2_775 ?
N18 Fe3 N18 81.6(5) 4_657 3_567 ?
N16 Fe4 N16 87.1(6) . 2_665 ?
N4 Fe4 N16 96.1(5) 2_665 2_665 ?
N4 Fe4 N16 87.5(5) 2_665 . ?
N4 Fe4 N16 87.5(5) . 2_665 ?
N4 Fe4 N16 96.1(5) . . ?
N4 Fe4 N4 175.0(6) . 2_665 ?
N3 Fe4 N16 172.4(5) 2_665 . ?
N3 Fe4 N16 87.6(4) 2_665 2_665 ?
N3 Fe4 N16 87.6(4) . . ?
N3 Fe4 N16 172.4(5) . 2_665 ?
N3 Fe4 N4 87.6(5) . . ?
N3 Fe4 N4 89.1(5) . 2_665 ?
N3 Fe4 N4 87.6(5) 2_665 2_665 ?
N3 Fe4 N4 89.1(5) 2_665 . ?
N3 Fe4 N3 98.2(6) . 2_665 ?
C1 N12 Fe1 153.6(12) . . ?
C9 N6 Fe2 174.0(13) . . ?
C14 N16 Fe4 152.1(11) . . ?
C2 N13 Fe1 175.1(13) . . ?
C10 N7 Fe2 159.5(11) . . ?
C11 N8 Fe2 179.4(13) . . ?
C12 N10 Fe3 177.0(13) . . ?
C3 N15 Fe3 177.6(13) . 1_445 ?
C4 N1 Fe1 178.0(11) . . ?
C8 N4 Fe4 178.0(11) . . ?
C5 N3 Fe4 178.2(13) . . ?
C13 N18 Fe3 161.3(10) . 3_467 ?
N12 C1 N11 172.1(14) . . ?
N13 C2 N14 171.5(14) . . ?
N10 C12 N9 172.1(15) . . ?
N8 C11 N9 169.9(14) . . ?
C3 N14 C2 124.4(12) . . ?
N1 C4 N2 170.9(15) . . ?
C11 N9 C12 125.3(13) . . ?
N15 C3 N14 170.3(15) . . ?
N4 C8 N5 170.2(16) . . ?
C5 N2 C4 122.0(13) . . ?
N6 C9 N5 171.4(15) . . ?
C8 N5 C9 124.1(13) . . ?
C1 N11 C10 118.4(12) . 3_466 ?
N7 C10 N11 173.5(14) . 3_566 ?
N3 C5 N2 170.1(15) . . ?
C60 N60 C69 106.5(11) . . ?
C60 N60 C65 112.3(14) . . ?
C60 N60 C73 114.8(14) . . ?
C65 N60 C69 106.7(12) . . ?
C73 N60 C69 111.8(13) . . ?
C73 N60 C65 104.5(13) . . ?
C62A C61 C60 120(2) . . ?
N60 C60 C61 119.5(15) . . ?
C67 C66 C65 113.7(18) . . ?
C40 N40 C48 103.9(10) . . ?
C52 N40 C48 110.9(13) . . ?
C52 N40 C40 112.4(12) . . ?
C52 N40 C44 106.7(12) . . ?
C44 N40 C48 111.0(12) . . ?
C44 N40 C40 112.0(14) . . ?
C61 C62A C63A 114(3) . . ?
N40 C48 C49 115.4(13) . . ?
C69 C70 C71B 106(3) . . ?
C69 C70 C71A 126(3) . . ?
C41 C40 N40 114.7(13) . . ?
C43A C42 C41 134(4) . . ?
C41 C42 C43B 103(4) . . ?
C70 C69 N60 117.1(15) . . ?
N60 C65 C66 114.8(15) . . ?
C54B C53 C52 96(3) . . ?
C54A C53 C52 114(3) . . ?
C49 C50A C51A 123(5) . . ?
N40 C52 C53 117.3(14) . . ?
C44 C45 C46 116(2) . . ?
C51B C50B C49 72(3) . . ?
C48 C49 C50B 102(2) . . ?
C48 C49 C51B 109(3) . . ?
C50A C49 C48 121(3) . . ?
C50B C49 C51B 49(2) . . ?
N40 C44 C45 115.1(15) . . ?
C53 C54B C55B 119(5) . . ?
C47 C46 C45 111(2) . . ?
C74 C73 N60 115.2(17) . . ?
C74 C75 C76 105(3) . 4 ?
C72 C71B C70 110(5) . . ?
C73 C74 C75 121(2) . . ?
N18 C13 N17 164(2) . . ?
N16 C14 N17 169.7(18) . . ?
C14 N17 C13 116.9(13) . . ?
C66 C67 C68 110(2) . . ?
C50B C51B C49 60(4) . . ?
C53 C54A C55A 109(3) . . ?
C42 C41 C40 112(2) . . ?
C63B C62B C61 101(4) . . ?
C72 C71A C70 114(5) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.93(3)
2 0.07(3)

