# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1-123K
_database_code_depnum_ccdc_archive 'CCDC 1569642'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H60 Co5 N30'
_chemical_formula_sum            'C54 H60 Co5 N30'
_chemical_formula_weight         1423.97
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.6215(15)
_cell_length_b                   15.6215(15)
_cell_length_c                   24.797(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5240.4(11)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    1468
_cell_measurement_temperature    123
_cell_measurement_theta_max      23.8250
_cell_measurement_theta_min      3.4311
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2187
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7245
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_min         3.122
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   ?
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1694
_reflns_number_total             2133
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+10.0728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0915
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(4) 0.50(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C4B \\sim N1-C4A
 with sigma of 0.02
 C3B-C4B \\sim C3A-C4A
 with sigma of 0.02
 N2B-C3B \\sim N2A-C3A
 with sigma of 0.02
 N2B-C2B \\sim N2A-C2A
 with sigma of 0.02
 C1B-C2B \\sim C1A-C2A
 with sigma of 0.02
 N1-C1B \\sim N1-C1A
 with sigma of 0.02
 N3-C5B \\sim N3-C5A
 with sigma of 0.02
 C4B-C5B \\sim C4A-C5A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C5B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5B) \\sim Ueq, Uanis(C5A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(C1B) = Uanis(C1A)
Uanis(C3B) = Uanis(C3A)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
5. Others
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C1B)=Sof(H1B)=Sof(C4B)=Sof(C2B)=Sof(H2B)=
 Sof(C3B)=Sof(H3B)=Sof(N2B)=1-FVAR(1)
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C4A)=Sof(C3A)=Sof(H3A)=Sof(N2A)=Sof(C2A)=
 Sof(H2A)=Sof(C1A)=Sof(H1A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C5B(H5BA,H5BB), C5A(H5AA,H5AB)
6.b Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C2B(H2B), C3B(H3B), C3A(H3A), C2A(H2A), C1A(H1A)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Co2 Co 0.3333 0.6667 0.80281(5) 0.0124(4) Uani 1 3 d S T P . .
Co1 Co 0.56996(7) 0.6667 0.6667 0.0176(3) Uani 1 2 d S T P A .
N3 N 0.7025(4) 0.7211(4) 0.71576(18) 0.0182(12) Uani 1 1 d D . . . .
C8 C 0.4396(5) 0.6883(5) 0.7577(2) 0.0168(15) Uani 1 1 d . . . . .
N4 N 0.4993(4) 0.6963(5) 0.7280(2) 0.0276(15) Uani 1 1 d . . . . .
C9 C 0.3598(5) 0.5816(5) 0.8461(2) 0.0190(16) Uani 1 1 d . . . . .
C7 C 0.7767(5) 0.7132(5) 0.6829(3) 0.0259(18) Uani 1 1 d . . . . .
H7A H 0.8279 0.7140 0.7068 0.031 Uiso 1 1 calc R . . . .
H7B H 0.8093 0.7708 0.6584 0.031 Uiso 1 1 calc R . . . .
C6 C 0.6862(5) 0.6666(5) 0.7666(2) 0.0284(18) Uani 1 1 d . . . . .
H6A H 0.6353 0.6705 0.7877 0.043 Uiso 1 1 calc GR . . . .
H6B H 0.7480 0.6958 0.7872 0.043 Uiso 1 1 calc GR . . . .
H6C H 0.6645 0.5973 0.7587 0.043 Uiso 1 1 calc GR . . . .
N5 N 0.3771(5) 0.5300(5) 0.8705(2) 0.0340(17) Uani 1 1 d . . . . .
N1 N 0.6529(4) 0.8210(4) 0.64457(19) 0.0283(14) Uani 1 1 d D . . . .
C5B C 0.722(3) 0.8197(16) 0.7343(11) 0.019(4) Uani 0.41(2) 1 d D U . A 2
H5BA H 0.7897 0.8584 0.7490 0.022 Uiso 0.41(2) 1 calc R . . A 2
H5BB H 0.6744 0.8122 0.7629 0.022 Uiso 0.41(2) 1 calc R . . A 2
C1B C 0.635(8) 0.858(3) 0.600(3) 0.042(4) Uani 0.41(2) 1 d D . . A 2
H1B H 0.5979 0.8183 0.5701 0.051 Uiso 0.41(2) 1 calc R . . A 2
C4B C 0.7099(19) 0.8704(18) 0.6862(8) 0.023(4) Uani 0.41(2) 1 d D . . A 2
C2B C 0.676(2) 0.962(2) 0.6013(11) 0.044(9) Uani 0.41(2) 1 d D . . A 2
H2B H 0.6538 0.9929 0.5767 0.053 Uiso 0.41(2) 1 calc R . . A 2
C3B C 0.760(2) 0.9715(18) 0.6788(11) 0.056(6) Uani 0.41(2) 1 d D . . A 2
H3B H 0.8079 1.0112 0.7051 0.068 Uiso 0.41(2) 1 calc R . . A 2
N2B N 0.747(2) 1.0166(17) 0.6374(10) 0.065(8) Uani 0.41(2) 1 d D . . A 2
C5A C 0.7431(19) 0.8289(10) 0.7240(8) 0.019(4) Uani 0.59(2) 1 d D U . A 1
H5AA H 0.8130 0.8598 0.7355 0.022 Uiso 0.59(2) 1 calc R . . A 1
H5AB H 0.7057 0.8394 0.7529 0.022 Uiso 0.59(2) 1 calc R . . A 1
C4A C 0.7367(12) 0.8772(13) 0.6730(6) 0.023(4) Uani 0.59(2) 1 d D . . A 1
C3A C 0.8103(18) 0.9725(12) 0.6601(7) 0.056(6) Uani 0.59(2) 1 d D . . A 1
H3A H 0.8660 1.0058 0.6832 0.068 Uiso 0.59(2) 1 calc R . . A 1
N2A N 0.8046(16) 1.0178(13) 0.6166(8) 0.075(7) Uani 0.59(2) 1 d D . . A 1
C2A C 0.7218(18) 0.9675(17) 0.5866(9) 0.058(7) Uani 0.59(2) 1 d D . . A 1
H2A H 0.7145 0.9958 0.5543 0.069 Uiso 0.59(2) 1 calc R . . A 1
C1A C 0.646(6) 0.873(2) 0.603(2) 0.042(4) Uani 0.59(2) 1 d D . . A 1
H1A H 0.5856 0.8434 0.5833 0.051 Uiso 0.59(2) 1 calc R . . A 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
Co2 C8 1.887(6) 2_665 ?
Co2 C8 1.887(6) 3_565 ?
Co2 C8 1.887(6) . ?
Co2 C9 1.907(7) 3_565 ?
Co2 C9 1.907(7) . ?
Co2 C9 1.907(7) 2_665 ?
Co1 N3 2.175(5) 10_566 ?
Co1 N3 2.175(5) . ?
Co1 N4 2.062(6) . ?
Co1 N4 2.062(6) 10_566 ?
Co1 N1 2.161(6) 10_566 ?
Co1 N1 2.161(6) . ?
N3 C7 1.471(8) . ?
N3 C6 1.469(8) . ?
N3 C5B 1.486(19) . ?
N3 C5A 1.487(14) . ?
C8 N4 1.146(7) . ?
C9 N5 1.144(8) . ?
C7 C7 1.494(13) 10_566 ?
N1 C1B 1.35(2) . ?
N1 C4B 1.330(19) . ?
N1 C4A 1.354(14) . ?
N1 C1A 1.347(14) . ?
C5B C4B 1.49(2) . ?
C1B C2B 1.41(4) . ?
C4B C3B 1.38(2) . ?
C2B N2B 1.34(2) . ?
C3B N2B 1.32(2) . ?
C5A C4A 1.499(14) . ?
C4A C3A 1.388(17) . ?
C3A N2A 1.319(16) . ?
N2A C2A 1.351(19) . ?
C2A C1A 1.42(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
C8 Co2 C8 88.5(3) 2_665 3_565 ?
C8 Co2 C8 88.5(3) 2_665 . ?
C8 Co2 C8 88.5(3) 3_565 . ?
C8 Co2 C9 177.3(3) 3_565 2_665 ?
C8 Co2 C9 88.9(3) . . ?
C8 Co2 C9 177.3(3) 2_665 . ?
C8 Co2 C9 91.2(3) . 2_665 ?
C8 Co2 C9 91.2(3) 2_665 3_565 ?
C8 Co2 C9 91.2(3) 3_565 . ?
C8 Co2 C9 88.9(3) 3_565 3_565 ?
C8 Co2 C9 177.3(3) . 3_565 ?
C8 Co2 C9 88.9(3) 2_665 2_665 ?
C9 Co2 C9 91.5(3) 3_565 . ?
C9 Co2 C9 91.5(3) 2_665 . ?
C9 Co2 C9 91.5(3) 3_565 2_665 ?
N3 Co1 N3 81.7(3) . 10_566 ?
N4 Co1 N3 90.7(2) . . ?
N4 Co1 N3 90.7(2) 10_566 10_566 ?
N4 Co1 N3 165.5(2) 10_566 . ?
N4 Co1 N3 165.5(2) . 10_566 ?
N4 Co1 N4 99.3(3) . 10_566 ?
N4 Co1 N1 91.6(2) . 10_566 ?
N4 Co1 N1 91.6(2) 10_566 . ?
N4 Co1 N1 91.5(2) . . ?
N4 Co1 N1 91.5(2) 10_566 10_566 ?
N1 Co1 N3 77.5(2) . . ?
N1 Co1 N3 98.8(2) 10_566 . ?
N1 Co1 N3 98.8(2) . 10_566 ?
N1 Co1 N3 77.5(2) 10_566 10_566 ?
N1 Co1 N1 175.2(3) 10_566 . ?
C7 N3 Co1 107.0(3) . . ?
C7 N3 C5B 119.9(16) . . ?
C7 N3 C5A 105.3(10) . . ?
C6 N3 Co1 113.4(4) . . ?
C6 N3 C7 110.0(5) . . ?
C6 N3 C5B 102.8(11) . . ?
C6 N3 C5A 113.0(8) . . ?
C5B N3 Co1 103.8(15) . . ?
C5A N3 Co1 107.6(10) . . ?
N4 C8 Co2 175.1(6) . . ?
C8 N4 Co1 161.4(6) . . ?
N5 C9 Co2 177.7(6) . . ?
N3 C7 C7 111.1(5) . 10_566 ?
C1B N1 Co1 123.4(19) . . ?
C4B N1 Co1 107.7(12) . . ?
C4B N1 C1B 128(2) . . ?
C4A N1 Co1 115.9(9) . . ?
C1A N1 Co1 132.8(15) . . ?
C1A N1 C4A 111(2) . . ?
N3 C5B C4B 107(2) . . ?
N1 C1B C2B 113(4) . . ?
N1 C4B C5B 122(2) . . ?
N1 C4B C3B 113(2) . . ?
C3B C4B C5B 124.2(18) . . ?
N2B C2B C1B 120(4) . . ?
N2B C3B C4B 124(3) . . ?
C3B N2B C2B 118(3) . . ?
N3 C5A C4A 110.9(14) . . ?
N1 C4A C5A 113.5(15) . . ?
N1 C4A C3A 126.0(16) . . ?
C3A C4A C5A 120.4(13) . . ?
N2A C3A C4A 121.5(18) . . ?
C3A N2A C2A 116.1(19) . . ?
N2A C2A C1A 121(2) . . ?
N1 C1A C2A 125(4) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(4)
2 0.50(4)
####################################################################### 
# 
# 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_2-100K
_database_code_depnum_ccdc_archive 'CCDC 1569643'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-04-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C54 H60 Co2.9 Fe2.1 N30)'
_chemical_formula_sum            'C54 H60 Co2.90 Fe2.10 N30'
_chemical_formula_weight         1417.47
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.5034(10)
_cell_length_b                   15.5034(10)
_cell_length_c                   24.835(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5169.6(8)
_cell_formula_units_Z            3.00006
_cell_measurement_reflns_used    2301
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.8289
_cell_measurement_theta_min      3.4501
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2181
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8468
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.358
_diffrn_reflns_theta_min         3.450
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   ?
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1820
_reflns_number_total             2117
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2117
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0340
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0407P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0754
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.48(3)
 0.52(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{Co1, Fe1}
4. Restrained distances
 N1-C4B \\sim N1-C4A
 with sigma of 0.02
 C3B-C4B \\sim C3A-C4A
 with sigma of 0.02
 N2B-C3B \\sim N2A-C3A
 with sigma of 0.02
 N2B-C2B \\sim N2A-C2A
 with sigma of 0.02
 C1B-C2B \\sim C1A-C2A
 with sigma of 0.02
 N1-C1B \\sim N1-C1A
 with sigma of 0.02
 N3-C5B \\sim N3-C5A
 with sigma of 0.02
 C4B-C5B \\sim C4A-C5A
 with sigma of 0.02
5. Restrained planarity
 N1, C5B, C1B, C4B, C2B, C3B, N2B
 with sigma of 0.1
 N1, C5A, C4A, C3A, N2A, C2A, C1A
 with sigma of 0.1
6. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(Fe1)
Uanis(C1B) = Uanis(C1A)
Uanis(C3B) = Uanis(C3A)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
7. Others
 Fixed Sof: Fe1(0.35) C5B(0.43) H5Ba(0.43) H5Bb(0.43) C1B(0.43) H1B(0.43)
 C4B(0.43) C2B(0.43) H2B(0.43) C3B(0.43) H3B(0.43) N2B(0.43) C5A(0.57)
 H5Aa(0.57) H5Ab(0.57) C4A(0.57) C3A(0.57) H3A(0.57) N2A(0.57) C2A(0.57)
 H2A(0.57) C1A(0.57) H1A(0.57) Co1(0.15)
8.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C5B(H5Ba,H5Bb), C5A(H5Aa,H5Ab)
8.b Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C2B(H2B), C3B(H3B), C3A(H3A), C2A(H2A), C1A(H1A)
8.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Co2 Co 0.3333 0.6667 0.79994(4) 0.0166(3) Uani 1 3 d S T P . .
Fe1 Fe 0.57246(5) 0.6667 0.6667 0.0173(2) Uani 0.7 2 d S T P A 1
N3 N 0.6991(3) 0.7163(3) 0.71637(16) 0.0227(9) Uani 1 1 d D . . . .
C8 C 0.4399(3) 0.6881(3) 0.7545(2) 0.0198(11) Uani 1 1 d . . . . .
N4 N 0.4989(3) 0.6941(3) 0.72454(18) 0.0283(10) Uani 1 1 d . . . . .
C9 C 0.3614(3) 0.5821(3) 0.8432(2) 0.0255(12) Uani 1 1 d . . . . .
C7 C 0.7766(3) 0.7122(4) 0.6840(2) 0.0272(12) Uani 1 1 d . . . . .
H7A H 0.8269 0.7111 0.7081 0.033 Uiso 1 1 calc R . . . .
H7B H 0.8106 0.7723 0.6610 0.033 Uiso 1 1 calc R . . . .
C6 C 0.6817(4) 0.6575(4) 0.7665(2) 0.0357(14) Uani 1 1 d . . . . .
H6A H 0.6267 0.6560 0.7867 0.054 Uiso 1 1 calc GR . . . .
H6B H 0.7421 0.6883 0.7886 0.054 Uiso 1 1 calc GR . . . .
H6C H 0.6647 0.5893 0.7572 0.054 Uiso 1 1 calc GR . . . .
N5 N 0.3811(4) 0.5313(3) 0.8679(2) 0.0400(12) Uani 1 1 d . . . . .
N1 N 0.6513(3) 0.8161(3) 0.64588(17) 0.0312(10) Uani 1 1 d D . . . .
C5B C 0.721(3) 0.8152(16) 0.7371(12) 0.028(4) Uani 0.43 1 d D . . A 2
H5BA H 0.7891 0.8526 0.7523 0.034 Uiso 0.43 1 calc R . . A 2
H5BB H 0.6724 0.8083 0.7650 0.034 Uiso 0.43 1 calc R . . A 2
C1B C 0.636(2) 0.854(3) 0.6010(11) 0.045(3) Uani 0.43 1 d D . . A 2
H1B H 0.5986 0.8146 0.5713 0.054 Uiso 0.43 1 calc R . . A 2
C4B C 0.7115(18) 0.8652(16) 0.6875(10) 0.036(4) Uani 0.43 1 d D . . A 2
C2B C 0.6808(16) 0.959(2) 0.6020(11) 0.053(8) Uani 0.43 1 d D . . A 2
H2B H 0.6615 0.9908 0.5760 0.064 Uiso 0.43 1 calc R . . A 2
C3B C 0.7605(14) 0.9694(15) 0.6800(9) 0.056(4) Uani 0.43 1 d D . . A 2
H3B H 0.8049 1.0099 0.7075 0.067 Uiso 0.43 1 calc R . . A 2
N2B N 0.7497(14) 1.0143(13) 0.6385(8) 0.068(6) Uani 0.43 1 d D . . A 2
C5A C 0.738(2) 0.8240(11) 0.7260(8) 0.028(4) Uani 0.57 1 d D . . A 1
H5AA H 0.8076 0.8556 0.7384 0.034 Uiso 0.57 1 calc R . . A 1
H5AB H 0.6979 0.8319 0.7548 0.034 Uiso 0.57 1 calc R . . A 1
C4A C 0.7324(11) 0.8753(12) 0.6759(6) 0.036(4) Uani 0.57 1 d D . . A 1
C3A C 0.8083(11) 0.9738(10) 0.6634(6) 0.056(4) Uani 0.57 1 d D . . A 1
H3A H 0.8636 1.0082 0.6869 0.067 Uiso 0.57 1 calc R . . A 1
N2A N 0.8021(11) 1.0175(10) 0.6193(6) 0.080(6) Uani 0.57 1 d D . . A 1
C2A C 0.7209(13) 0.9645(16) 0.5889(9) 0.063(7) Uani 0.57 1 d D . . A 1
H2A H 0.7136 0.9924 0.5563 0.076 Uiso 0.57 1 calc R . . A 1
C1A C 0.6458(18) 0.8677(19) 0.6044(8) 0.045(3) Uani 0.57 1 d D . . A 1
H1A H 0.5865 0.8370 0.5835 0.054 Uiso 0.57 1 calc R . . A 1
Co1 Co 0.57246(5) 0.6667 0.6667 0.0173(2) Uani 0.3 2 d S T 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
Co2 C8 1.889(5) 2_665 ?
Co2 C8 1.889(5) 3_565 ?
Co2 C8 1.889(5) . ?
Co2 C9 1.906(5) 3_565 ?
Co2 C9 1.906(5) . ?
Co2 C9 1.906(5) 2_665 ?
Fe1 N3 2.112(4) 10_566 ?
Fe1 N3 2.112(4) . ?
Fe1 N4 2.008(4) . ?
Fe1 N4 2.008(4) 10_566 ?
Fe1 N1 2.073(4) . ?
Fe1 N1 2.073(4) 10_566 ?
N3 C7 1.473(6) . ?
N3 C6 1.485(6) . ?
N3 C5B 1.488(18) . ?
N3 C5A 1.485(14) . ?
N3 Co1 2.112(4) . ?
C8 N4 1.146(6) . ?
N4 Co1 2.008(4) . ?
C9 N5 1.152(6) . ?
C7 C7 1.493(10) 10_566 ?
N1 C1B 1.337(19) . ?
N1 C4B 1.344(18) . ?
N1 C4A 1.350(14) . ?
N1 C1A 1.334(14) . ?
N1 Co1 2.073(4) . ?
C5B C4B 1.503(19) . ?
C1B C2B 1.41(2) . ?
C4B C3B 1.41(2) . ?
C2B N2B 1.33(2) . ?
C3B N2B 1.301(18) . ?
C5A C4A 1.501(14) . ?
C4A C3A 1.420(15) . ?
C3A N2A 1.316(15) . ?
N2A C2A 1.341(16) . ?
C2A C1A 1.417(17) . ?
Co1 N3 2.112(4) 10_566 ?
Co1 N4 2.008(4) 10_566 ?
Co1 N1 2.073(4) 10_566 ?

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
C8 Co2 C8 87.9(2) 2_665 3_565 ?
C8 Co2 C8 87.9(2) 2_665 . ?
C8 Co2 C8 87.9(2) 3_565 . ?
C8 Co2 C9 92.0(2) . 2_665 ?
C8 Co2 C9 88.7(2) 2_665 2_665 ?
C8 Co2 C9 92.04(19) 3_565 . ?
C8 Co2 C9 92.04(19) 2_665 3_565 ?
C8 Co2 C9 176.7(2) 3_565 2_665 ?
C8 Co2 C9 176.7(2) . 3_565 ?
C8 Co2 C9 88.7(2) . . ?
C8 Co2 C9 176.7(2) 2_665 . ?
C8 Co2 C9 88.7(2) 3_565 3_565 ?
C9 Co2 C9 91.3(2) 3_565 . ?
C9 Co2 C9 91.3(2) 2_665 . ?
C9 Co2 C9 91.3(2) 3_565 2_665 ?
N3 Fe1 N3 83.2(2) . 10_566 ?
N4 Fe1 N3 91.60(15) 10_566 10_566 ?
N4 Fe1 N3 168.49(16) . 10_566 ?
N4 Fe1 N3 168.50(17) 10_566 . ?
N4 Fe1 N3 91.59(15) . . ?
N4 Fe1 N4 95.3(2) . 10_566 ?
N4 Fe1 N1 91.25(17) 10_566 10_566 ?
N4 Fe1 N1 91.25(17) . . ?
N4 Fe1 N1 91.15(16) . 10_566 ?
N4 Fe1 N1 91.15(16) 10_566 . ?
N1 Fe1 N3 79.46(16) 10_566 10_566 ?
N1 Fe1 N3 97.84(16) . 10_566 ?
N1 Fe1 N3 79.46(16) . . ?
N1 Fe1 N3 97.84(16) 10_566 . ?
N1 Fe1 N1 176.4(2) . 10_566 ?
C7 N3 Fe1 107.1(3) . . ?
C7 N3 C6 109.5(4) . . ?
C7 N3 C5B 117.6(17) . . ?
C7 N3 C5A 105.0(12) . . ?
C7 N3 Co1 107.1(3) . . ?
C6 N3 Fe1 114.5(3) . . ?
C6 N3 C5B 102.7(12) . . ?
C6 N3 Co1 114.5(3) . . ?
C5B N3 Co1 105.6(17) . . ?
C5A N3 Fe1 106.3(12) . . ?
C5A N3 C6 113.7(8) . . ?
N4 C8 Co2 174.2(4) . . ?
C8 N4 Fe1 164.2(4) . . ?
C8 N4 Co1 164.2(4) . . ?
N5 C9 Co2 177.2(5) . . ?
N3 C7 C7 110.2(3) . 10_566 ?
C1B N1 C4B 128(2) . . ?
C1B N1 Co1 124.5(18) . . ?
C4B N1 Co1 107.2(11) . . ?
C4A N1 Fe1 116.8(9) . . ?
C1A N1 Fe1 133.1(13) . . ?
C1A N1 C4A 109.6(15) . . ?
N3 C5B C4B 102.5(19) . . ?
N1 C1B C2B 114(3) . . ?
N1 C4B C5B 124(2) . . ?
N1 C4B C3B 112(2) . . ?
C3B C4B C5B 124.2(18) . . ?
N2B C2B C1B 122(3) . . ?
N2B C3B C4B 125(2) . . ?
C3B N2B C2B 118(2) . . ?
N3 C5A C4A 111.4(15) . . ?
N1 C4A C5A 112.1(17) . . ?
N1 C4A C3A 126.9(15) . . ?
C3A C4A C5A 121.1(13) . . ?
N2A C3A C4A 120.1(15) . . ?
C3A N2A C2A 116.2(16) . . ?
N2A C2A C1A 121(2) . . ?
N1 C1A C2A 125(2) . . ?
N3 Co1 N3 83.2(2) . 10_566 ?
N4 Co1 N3 91.59(15) . . ?
N4 Co1 N3 168.49(16) . 10_566 ?
N4 Co1 N3 91.60(15) 10_566 10_566 ?
N4 Co1 N3 168.50(17) 10_566 . ?
N4 Co1 N4 95.3(2) . 10_566 ?
N4 Co1 N1 91.15(16) . 10_566 ?
N4 Co1 N1 91.25(17) . . ?
N4 Co1 N1 91.15(16) 10_566 . ?
N4 Co1 N1 91.25(17) 10_566 10_566 ?
N1 Co1 N3 79.46(16) . . ?
N1 Co1 N3 97.84(16) . 10_566 ?
N1 Co1 N3 79.46(16) 10_566 10_566 ?
N1 Co1 N3 97.84(16) 10_566 . ?
N1 Co1 N1 176.4(2) . 10_566 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.48(3)
2 0.52(3)
####################################################################### 
# 
# 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_2_298K
_database_code_depnum_ccdc_archive 'CCDC 1569644'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-10-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C54 H60 Co2.9 Fe2.1 N30)'
_chemical_formula_sum            'C54 H60 Co2.90 Fe2.10 N30'
_chemical_formula_weight         1417.47
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.6964(15)
_cell_length_b                   15.6964(15)
_cell_length_c                   24.965(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5326.7(12)
_cell_formula_units_Z            3.00006
_cell_measurement_reflns_used    1520
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.0779
_cell_measurement_theta_min      3.4132
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2181
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7090
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         3.413
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   ?
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1424
_reflns_number_total             2177
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2177
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      0.989
_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)+(0.0580P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1225
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(6)
 0.50(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{Fe1, Co1}
4. Restrained distances
 C1B-C17B \\sim C1A-C17A
 with sigma of 0.02
 N3-C17B \\sim N3-C17A
 with sigma of 0.02
 N3-C15A \\sim C15A-C13A \\sim N2A-C13A \\sim N2A-C1A \\sim C1A-C17A \\sim
N3-C17A
 with sigma of 0.01
 C17A-C1 \\sim C17B-C1
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
N3 \\sim C13B \\sim C15B \\sim C17B \\sim C1B \\sim N2B: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N3 \\sim C15A \\sim C13A \\sim N2A \\sim C1A \\sim C17A: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(Fe1) = Uanis(Co1)
Uanis(C17A) = Uanis(C17B)
Uanis(C1A) = Uanis(C1B)
Uanis(C13A) = Uanis(C13B)
Uanis(C15A) = Uanis(C15B)
Uanis(N2A) = Uanis(N2B)
6. Others
 Fixed Sof: Fe1(0.35) C13B(0.59) H13B(0.59) C15B(0.59) H15B(0.59) C17B(0.59)
 C1B(0.59) H1B(0.59) N2B(0.59) C15A(0.41) H15A(0.41) C13A(0.41) H13A(0.41)
 N2A(0.41) C1A(0.41) H1A(0.41) C17A(0.41) H1BC(0.59) H1BD(0.59) H1AA(0.41)
 H1AB(0.41) Co1(0.15)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C1(H1BC,H1BD), C1(H1AA,H1AB)
7.b Aromatic/amide H refined with riding coordinates:
 C13B(H13B), C15B(H15B), C1B(H1B), C15A(H15A), C13A(H13A), C1A(H1A)
7.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 -0.43051(8) -0.333333 -0.333333 0.0386(4) Uani 0.7 2 d S T P A 1
Co2 Co -0.666667 -0.333333 -0.46749(7) 0.0364(5) Uani 1 3 d S T P . .
N3 N -0.3482(5) -0.1806(5) -0.3550(3) 0.0580(18) Uani 1 1 d D U . . .
N4 N -0.2995(5) -0.2810(5) -0.2850(3) 0.0484(17) Uani 1 1 d . . . . .
N5 N -0.7096(7) -0.5118(7) -0.5353(4) 0.082(3) Uani 1 1 d . . . . .
N6 N -0.5299(6) -0.3610(6) -0.3936(3) 0.059(2) Uani 1 1 d . . . . .
C7 C -0.6921(6) -0.4424(7) -0.5104(4) 0.050(2) Uani 1 1 d . . . . .
C8 C -0.5823(5) -0.3533(5) -0.4234(3) 0.0390(19) Uani 1 1 d . . . . .
C9 C -0.3157(8) -0.3359(8) -0.2336(4) 0.074(3) Uani 1 1 d . . . . .
H9A H -0.332955 -0.402600 -0.241209 0.111 Uiso 1 1 calc GR . . . .
H9B H -0.368056 -0.335437 -0.213987 0.111 Uiso 1 1 calc GR . . . .
H9C H -0.256520 -0.304972 -0.212647 0.111 Uiso 1 1 calc GR . . . .
C11 C -0.2245(6) -0.2874(7) -0.3176(4) 0.057(3) Uani 1 1 d . . . . .
H11A H -0.174121 -0.285755 -0.294452 0.069 Uiso 1 1 calc R . . . .
H11B H -0.193501 -0.231366 -0.341629 0.069 Uiso 1 1 calc R . . . .
C13B C -0.284(2) -0.035(3) -0.4113(14) 0.109(11) Uani 0.59 1 d . U . A 2
H13B H -0.293637 -0.006551 -0.441712 0.131 Uiso 0.59 1 calc R . . A 2
C15B C -0.361(9) -0.135(4) -0.396(2) 0.082(6) Uani 0.59 1 d . U . A 2
H15B H -0.419168 -0.165830 -0.415713 0.099 Uiso 0.59 1 calc R . . A 2
C17B C -0.2663(15) -0.1279(12) -0.3251(7) 0.057(6) Uani 0.59 1 d D U . A 2
C1B C -0.196(2) -0.0299(14) -0.3394(10) 0.101(9) Uani 0.59 1 d D U . A 2
H1B H -0.142092 0.003662 -0.316591 0.122 Uiso 0.59 1 calc R . . A 2
N2B N -0.1992(17) 0.0178(16) -0.3820(10) 0.120(9) Uani 0.59 1 d . U . A 2
C15A C -0.361(12) -0.141(5) -0.400(3) 0.082(6) Uani 0.41 1 d D U . A 1
H15A H -0.393555 -0.177713 -0.429992 0.099 Uiso 0.41 1 calc R . . A 1
C13A C -0.322(4) -0.042(5) -0.397(2) 0.109(11) Uani 0.41 1 d D U . A 1
H13A H -0.342155 -0.012158 -0.422373 0.131 Uiso 0.41 1 calc R . . A 1
N2A N -0.255(3) 0.014(2) -0.3605(14) 0.120(9) Uani 0.41 1 d D U . A 1
C1A C -0.232(3) -0.0244(19) -0.3186(14) 0.101(9) Uani 0.41 1 d D U . A 1
H1A H -0.182585 0.013203 -0.294134 0.122 Uiso 0.41 1 calc R . . A 1
C17A C -0.289(3) -0.1237(14) -0.3154(10) 0.057(6) Uani 0.41 1 d D U . A 1
C1 C -0.2670(8) -0.1761(7) -0.2718(4) 0.073(3) Uani 1 1 d D . . . .
H1BC H -0.201797 -0.143957 -0.255925 0.087 Uiso 0.59 1 calc R . . A 2
H1BD H -0.312302 -0.172261 -0.246802 0.087 Uiso 0.59 1 calc R . . A 2
H1AA H -0.196713 -0.141319 -0.264938 0.087 Uiso 0.41 1 calc R . . A 1
H1AB H -0.299587 -0.174184 -0.239151 0.087 Uiso 0.41 1 calc R . . A 1
Co1 Co -0.43051(8) -0.333333 -0.333333 0.0386(4) Uani 0.3 2 d S T 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 2.148(7) . ?
Fe1 N3 2.148(7) 10_444 ?
Fe1 N4 2.162(6) 10_444 ?
Fe1 N4 2.162(6) . ?
Fe1 N6 2.051(8) 10_444 ?
Fe1 N6 2.051(8) . ?
Co2 C7 1.886(9) . ?
Co2 C7 1.885(9) 3_445 ?
Co2 C7 1.885(9) 2_455 ?
Co2 C8 1.865(9) 2_455 ?
Co2 C8 1.865(9) 3_445 ?
Co2 C8 1.865(9) . ?
N3 C15B 1.33(3) . ?
N3 C17B 1.353(16) . ?
N3 C15A 1.348(17) . ?
N3 C17A 1.345(14) . ?
N3 Co1 2.148(7) . ?
N4 C9 1.494(11) . ?
N4 C11 1.475(10) . ?
N4 C1 1.497(12) . ?
N4 Co1 2.162(6) . ?
N5 C7 1.160(10) . ?
N6 C8 1.159(9) . ?
N6 Co1 2.051(8) . ?
C11 C11 1.476(17) 10_444 ?
C13B C15B 1.46(7) . ?
C13B N2B 1.38(3) . ?
C17B C1B 1.42(2) . ?
C17B C1 1.529(18) . ?
C1B N2B 1.32(3) . ?
C15A C13A 1.348(17) . ?
C13A N2A 1.348(17) . ?
N2A C1A 1.342(17) . ?
C1A C17A 1.357(15) . ?
C17A C1 1.50(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 Fe1 N3 175.0(4) . 10_444 ?
N3 Fe1 N4 77.8(3) 10_444 10_444 ?
N3 Fe1 N4 98.3(3) 10_444 . ?
N3 Fe1 N4 98.3(3) . 10_444 ?
N3 Fe1 N4 77.8(3) . . ?
N4 Fe1 N4 80.8(4) 10_444 . ?
N6 Fe1 N3 91.2(3) 10_444 10_444 ?
N6 Fe1 N3 92.0(3) 10_444 . ?
N6 Fe1 N3 92.0(3) . 10_444 ?
N6 Fe1 N3 91.2(3) . . ?
N6 Fe1 N4 165.6(3) 10_444 10_444 ?
N6 Fe1 N4 165.6(3) . . ?
N6 Fe1 N4 91.7(3) . 10_444 ?
N6 Fe1 N4 91.7(3) 10_444 . ?
N6 Fe1 N6 98.2(4) 10_444 . ?
C7 Co2 C7 90.9(4) 3_445 2_455 ?
C7 Co2 C7 90.9(4) 2_455 . ?
C7 Co2 C7 90.9(4) 3_445 . ?
C8 Co2 C7 91.6(3) . . ?
C8 Co2 C7 88.8(4) 3_445 . ?
C8 Co2 C7 177.5(4) 2_455 . ?
C8 Co2 C7 88.8(4) . 2_455 ?
C8 Co2 C7 91.6(3) 2_455 2_455 ?
C8 Co2 C7 177.5(4) . 3_445 ?
C8 Co2 C7 177.5(4) 3_445 2_455 ?
C8 Co2 C7 91.6(3) 3_445 3_445 ?
C8 Co2 C7 88.8(3) 2_455 3_445 ?
C8 Co2 C8 88.7(3) 2_455 3_445 ?
C8 Co2 C8 88.7(3) 3_445 . ?
C8 Co2 C8 88.7(3) 2_455 . ?
C15B N3 C17B 117(4) . . ?
C15B N3 Co1 129(3) . . ?
C17B N3 Co1 113.7(8) . . ?
C15A N3 Fe1 126(4) . . ?
C17A N3 Fe1 112.8(11) . . ?
C17A N3 C15A 121(4) . . ?
C9 N4 Fe1 113.9(6) . . ?
C9 N4 C1 108.2(7) . . ?
C9 N4 Co1 113.9(6) . . ?
C11 N4 Fe1 107.8(5) . . ?
C11 N4 C9 110.3(7) . . ?
C11 N4 C1 110.6(7) . . ?
C11 N4 Co1 107.8(5) . . ?
C1 N4 Fe1 106.1(5) . . ?
C1 N4 Co1 106.1(5) . . ?
C8 N6 Fe1 162.4(7) . . ?
C8 N6 Co1 162.4(7) . . ?
N5 C7 Co2 177.4(9) . . ?
N6 C8 Co2 175.2(8) . . ?
N4 C11 C11 110.1(6) . 10_444 ?
N2B C13B C15B 123(4) . . ?
N3 C15B C13B 121(7) . . ?
N3 C17B C1B 120.8(17) . . ?
N3 C17B C1 114.1(13) . . ?
C1B C17B C1 124.3(15) . . ?
N2B C1B C17B 126(2) . . ?
C1B N2B C13B 113(3) . . ?
N3 C15A C13A 114(6) . . ?
N2A C13A C15A 123(7) . . ?
C1A N2A C13A 122(4) . . ?
N2A C1A C17A 113(3) . . ?
N3 C17A C1A 124(2) . . ?
N3 C17A C1 116.1(15) . . ?
C1A C17A C1 118.2(19) . . ?
N4 C1 C17B 105.5(9) . . ?
N4 C1 C17A 113.3(10) . . ?
N3 Co1 N3 175.0(4) . 10_444 ?
N3 Co1 N4 77.8(3) 10_444 10_444 ?
N3 Co1 N4 98.3(3) . 10_444 ?
N3 Co1 N4 98.3(3) 10_444 . ?
N3 Co1 N4 77.8(3) . . ?
N4 Co1 N4 80.8(4) 10_444 . ?
N6 Co1 N3 92.0(3) 10_444 . ?
N6 Co1 N3 91.2(3) 10_444 10_444 ?
N6 Co1 N3 91.2(3) . . ?
N6 Co1 N3 92.0(3) . 10_444 ?
N6 Co1 N4 91.7(3) 10_444 . ?
N6 Co1 N4 165.6(3) 10_444 10_444 ?
N6 Co1 N4 165.6(3) . . ?
N6 Co1 N4 91.7(3) . 10_444 ?
N6 Co1 N6 98.2(4) 10_444 . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(6)
2 0.50(6)

