# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1835922'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H9 O4, C57 H33 N12 Fe, C8 H20 O2, H2 O'
_chemical_formula_sum            'C65 H64 Fe N12 O7'
_chemical_formula_weight         1181.13

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P31

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   16.9172(2)
_cell_length_b                   16.9172(2)
_cell_length_c                   17.9975(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4460.66(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    11806
_cell_measurement_theta_min      2.9570
_cell_measurement_theta_max      73.4160

_exptl_crystal_description       cubic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1860
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.749
_oxdiff_exptl_absorpt_empirical_full_max 1.216
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33065
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         73.55
_reflns_number_total             10971
_reflns_number_gt                10111
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0661P)²+0.3008P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         10971
_refine_ls_number_parameters     781
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.009

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.88825(16) 0.32773(16) 0.03056(15) 0.0287(5) Uani 1 1 d . . .
H1 H 0.9291 0.3856 0.0487 0.034 Uiso 1 1 calc R . .
C2 C 0.80455(17) 0.27576(17) 0.06712(16) 0.0312(5) Uani 1 1 d . . .
H2 H 0.7912 0.2988 0.1092 0.037 Uiso 1 1 calc R . .
C3 C 0.74199(16) 0.19045(17) 0.04059(15) 0.0293(5) Uani 1 1 d . . .
H3 H 0.6863 0.1554 0.0645 0.035 Uiso 1 1 calc R . .
C4 C 0.76396(15) 0.15780(16) -0.02299(15) 0.0263(5) Uani 1 1 d . . .
C5 C 0.85003(16) 0.21258(15) -0.05587(14) 0.0241(5) Uani 1 1 d . . .
C6 C 0.87949(16) 0.18357(16) -0.11963(14) 0.0243(5) Uani 1 1 d . . .
C7 C 0.82422(16) 0.09704(16) -0.15245(15) 0.0271(5) Uani 1 1 d . . .
C8 C 0.85735(18) 0.07545(17) -0.21612(15) 0.0309(5) Uani 1 1 d . . .
H8 H 0.8225 0.0199 -0.2402 0.037 Uiso 1 1 calc R . .
C9 C 0.94221(17) 0.13788(17) -0.24222(16) 0.0320(5) Uani 1 1 d . . .
H9 H 0.9653 0.1245 -0.2842 0.038 Uiso 1 1 calc R . .
C10 C 0.99391(16) 0.22103(16) -0.20631(15) 0.0297(5) Uani 1 1 d . . .
H10 H 1.0516 0.2618 -0.2247 0.036 Uiso 1 1 calc R . .
C11 C 0.70778(16) 0.07129(17) -0.05765(15) 0.0295(5) Uani 1 1 d . . .
C12 C 0.73789(17) 0.04108(16) -0.11782(15) 0.0293(5) Uani 1 1 d . . .
C13 C 0.60178(17) -0.06517(18) -0.08771(18) 0.0345(6) Uani 1 1 d . . .
C14 C 0.51485(19) -0.15187(19) -0.08776(19) 0.0396(6) Uani 1 1 d . . .
C15 C 0.4352(2) -0.1555(2) -0.06342(19) 0.0496(8) Uani 1 1 d . . .
H15 H 0.4367 -0.1026 -0.0473 0.059 Uiso 1 1 calc R . .
C16 C 0.3535(2) -0.2378(3) -0.0630(2) 0.0651(12) Uani 1 1 d . . .
H16 H 0.3008 -0.2399 -0.0456 0.078 Uiso 1 1 calc R . .
C17 C 0.3499(3) -0.3167(3) -0.0882(3) 0.0709(12) Uani 1 1 d . . .
H17 H 0.2948 -0.3715 -0.0888 0.085 Uiso 1 1 calc R . .
C18 C 0.4289(3) -0.3133(2) -0.1126(2) 0.0631(11) Uani 1 1 d . . .
H18 H 0.4270 -0.3662 -0.1292 0.076 Uiso 1 1 calc R . .
C19 C 0.5112(2) -0.2315(2) -0.11237(19) 0.0478(8) Uani 1 1 d . . .
H19 H 0.5640 -0.2300 -0.1288 0.057 Uiso 1 1 calc R . .
C20 C 1.05365(16) 0.25330(16) 0.03064(15) 0.0295(5) Uani 1 1 d . . .
H20 H 0.9963 0.2382 0.0486 0.035 Uiso 1 1 calc R . .
C21 C 1.10282(18) 0.21871(18) 0.06710(16) 0.0332(6) Uani 1 1 d . . .
H21 H 1.0785 0.1818 0.1088 0.040 Uiso 1 1 calc R . .
C22 C 1.18715(17) 0.23960(18) 0.04105(15) 0.0303(5) Uani 1 1 d . . .
H22 H 1.2202 0.2165 0.0647 0.036 Uiso 1 1 calc R . .
C23 C 1.22357(16) 0.29632(16) -0.02188(15) 0.0267(5) Uani 1 1 d . . .
C24 C 1.16957(15) 0.32843(15) -0.05465(14) 0.0241(5) Uani 1 1 d . . .
C25 C 1.20006(15) 0.38655(15) -0.11907(14) 0.0239(5) Uani 1 1 d . . .
C26 C 1.28585(16) 0.41497(16) -0.15137(15) 0.0260(5) Uani 1 1 d . . .
C27 C 1.30893(16) 0.47188(16) -0.21408(15) 0.0290(5) Uani 1 1 d . . .
H27 H 1.3649 0.4927 -0.2375 0.035 Uiso 1 1 calc R . .
C28 C 1.24789(17) 0.49651(17) -0.24045(16) 0.0312(5) Uani 1 1 d . . .
H28 H 1.2628 0.5344 -0.2818 0.037 Uiso 1 1 calc R . .
C29 C 1.16406(16) 0.46495(16) -0.20552(15) 0.0283(5) Uani 1 1 d . . .
H29 H 1.1237 0.4822 -0.2243 0.034 Uiso 1 1 calc R . .
C30 C 1.30912(16) 0.32376(16) -0.05588(15) 0.0279(5) Uani 1 1 d . . .
C31 C 1.34049(16) 0.38205(17) -0.11740(15) 0.0274(5) Uani 1 1 d . . .
C32 C 1.43887(17) 0.34248(17) -0.08860(16) 0.0312(6) Uani 1 1 d . . .
C33 C 1.52085(17) 0.33327(19) -0.09190(18) 0.0346(6) Uani 1 1 d . . .
C34 C 1.5257(2) 0.2670(2) -0.04979(19) 0.0423(7) Uani 1 1 d . . .
H34 H 1.4773 0.2293 -0.0189 0.051 Uiso 1 1 calc R . .
C35 C 1.6017(2) 0.2560(3) -0.0530(2) 0.0545(9) Uani 1 1 d . . .
H35 H 1.6038 0.2113 -0.0244 0.065 Uiso 1 1 calc R . .
C36 C 1.6735(2) 0.3112(3) -0.0983(2) 0.0572(9) Uani 1 1 d . . .
H36 H 1.7245 0.3042 -0.1006 0.069 Uiso 1 1 calc R . .
C37 C 1.6698(2) 0.3777(3) -0.1408(2) 0.0520(8) Uani 1 1 d . . .
H37 H 1.7183 0.4150 -0.1718 0.062 Uiso 1 1 calc R . .
C38 C 1.59408(19) 0.3889(2) -0.13724(19) 0.0428(7) Uani 1 1 d . . .
H38 H 1.5924 0.4340 -0.1655 0.051 Uiso 1 1 calc R . .
C39 C 1.13167(16) 0.49742(16) 0.02937(14) 0.0277(5) Uani 1 1 d . . .
H39 H 1.1494 0.4572 0.0477 0.033 Uiso 1 1 calc R . .
C40 C 1.16315(17) 0.58111(17) 0.06504(16) 0.0317(5) Uani 1 1 d . . .
H40 H 1.2006 0.5956 0.1066 0.038 Uiso 1 1 calc R . .
C41 C 1.13865(17) 0.64231(17) 0.03868(15) 0.0307(5) Uani 1 1 d . . .
H41 H 1.1594 0.6982 0.0622 0.037 Uiso 1 1 calc R . .
C42 C 1.08198(16) 0.61954(16) -0.02416(15) 0.0264(5) Uani 1 1 d . . .
C43 C 1.05342(15) 0.53328(15) -0.05623(14) 0.0238(5) Uani 1 1 d . . .
C44 C 0.99509(15) 0.50294(15) -0.12093(14) 0.0260(5) Uani 1 1 d . . .
C45 C 0.96293(16) 0.55667(16) -0.15354(15) 0.0264(5) Uani 1 1 d . . .
C46 C 0.90675(18) 0.52091(18) -0.21657(15) 0.0317(5) Uani 1 1 d . . .
H46 H 0.8841 0.5543 -0.2403 0.038 Uiso 1 1 calc R . .
C47 C 0.88555(19) 0.43617(19) -0.24273(16) 0.0343(6) Uani 1 1 d . . .
H47 H 0.8486 0.4119 -0.2844 0.041 Uiso 1 1 calc R . .
C48 C 0.91978(17) 0.38694(16) -0.20647(15) 0.0283(5) Uani 1 1 d . . .
H48 H 0.9046 0.3295 -0.2245 0.034 Uiso 1 1 calc R . .
C49 C 1.04887(16) 0.67363(16) -0.05816(15) 0.0281(5) Uani 1 1 d . . .
C50 C 0.99036(16) 0.64274(16) -0.12009(15) 0.0261(5) Uani 1 1 d . . .
C51 C 1.00915(17) 0.77219(17) -0.08719(15) 0.0304(6) Uani 1 1 d . . .
C52 C 0.99986(19) 0.85405(17) -0.08368(18) 0.0351(6) Uani 1 1 d . . .
C53 C 1.0556(2) 0.92740(19) -0.03828(19) 0.0422(7) Uani 1 1 d . . .
H53 H 1.1007 0.9258 -0.0099 0.051 Uiso 1 1 calc R . .
C54 C 1.0443(3) 1.0030(2) -0.0350(2) 0.0523(8) Uani 1 1 d . . .
H54 H 1.0817 1.0517 -0.0042 0.063 Uiso 1 1 calc R . .
C55 C 0.9777(3) 1.0067(2) -0.0771(2) 0.0585(9) Uani 1 1 d . . .
H55 H 0.9703 1.0575 -0.0748 0.070 Uiso 1 1 calc R . .
C56 C 0.9229(3) 0.9348(2) -0.1224(2) 0.0537(8) Uani 1 1 d . . .
H56 H 0.8784 0.9370 -0.1511 0.064 Uiso 1 1 calc R . .
C57 C 0.9333(2) 0.8588(2) -0.12568(19) 0.0415(7) Uani 1 1 d . . .
H57 H 0.8954 0.8102 -0.1564 0.050 Uiso 1 1 calc R . .
C61 C 0.8505(3) 0.0279(3) 0.0917(3) 0.0824(15) Uani 1 1 d . . .
H61A H 0.7972 -0.0318 0.0917 0.124 Uiso 1 1 calc R . .
H61B H 0.9042 0.0223 0.0942 0.124 Uiso 1 1 calc R . .
H61C H 0.8518 0.0594 0.0470 0.124 Uiso 1 1 calc R . .
C62 C 0.8477(3) 0.0808(3) 0.1580(3) 0.0730(13) Uani 1 1 d . . .
H62A H 0.7931 0.0858 0.1560 0.088 Uiso 1 1 calc R . .
H62B H 0.8458 0.0489 0.2033 0.088 Uiso 1 1 calc R . .
C63 C 0.9306(3) 0.2237(3) 0.2204(2) 0.0703(11) Uani 1 1 d . . .
H63A H 0.9314 0.1938 0.2661 0.084 Uiso 1 1 calc R . .
H63B H 0.8771 0.2308 0.2210 0.084 Uiso 1 1 calc R . .
C64 C 1.0148(4) 0.3155(4) 0.2157(3) 0.0890(16) Uani 1 1 d . . .
H64A H 1.0170 0.3518 0.2576 0.133 Uiso 1 1 calc R . .
H64B H 1.0136 0.3453 0.1706 0.133 Uiso 1 1 calc R . .
H64C H 1.0677 0.3085 0.2160 0.133 Uiso 1 1 calc R . .
C65 C 0.6943(3) 0.1840(3) 0.7328(3) 0.0825(15) Uani 1 1 d . . .
H65A H 0.6347 0.1306 0.7328 0.124 Uiso 1 1 calc R . .
H65B H 0.6885 0.2375 0.7300 0.124 Uiso 1 1 calc R . .
H65C H 0.7258 0.1856 0.7776 0.124 Uiso 1 1 calc R . .
C66 C 0.7477(3) 0.1811(3) 0.6664(3) 0.0739(13) Uani 1 1 d . . .
H66A H 0.7527 0.1265 0.6686 0.089 Uiso 1 1 calc R . .
H66B H 0.7158 0.1791 0.6210 0.089 Uiso 1 1 calc R . .
C67 C 0.8901(3) 0.2640(3) 0.6037(2) 0.0723(12) Uani 1 1 d . . .
H67A H 0.8600 0.2651 0.5581 0.087 Uiso 1 1 calc R . .
H67B H 0.8970 0.2105 0.6026 0.087 Uiso 1 1 calc R . .
C68 C 0.9821(4) 0.3482(4) 0.6084(3) 0.0900(16) Uani 1 1 d . . .
H68A H 1.0182 0.3508 0.5664 0.135 Uiso 1 1 calc R . .
H68B H 1.0119 0.3466 0.6533 0.135 Uiso 1 1 calc R . .
H68C H 0.9751 0.4011 0.6087 0.135 Uiso 1 1 calc R . .
N1 N 0.91149(13) 0.29736(13) -0.02919(13) 0.0251(4) Uani 1 1 d . . .
N2 N 0.96390(13) 0.24480(13) -0.14615(13) 0.0248(4) Uani 1 1 d . . .
N3 N 0.62063(14) 0.00352(15) -0.03961(13) 0.0324(5) Uani 1 1 d . . .
N4 N 0.67027(15) -0.04615(14) -0.13541(13) 0.0326(5) Uani 1 1 d . . .
N5 N 1.08567(13) 0.30689(13) -0.02877(12) 0.0251(4) Uani 1 1 d . . .
N6 N 1.13956(13) 0.41073(13) -0.14593(12) 0.0251(4) Uani 1 1 d . . .
N7 N 1.37209(14) 0.29839(15) -0.03777(13) 0.0297(5) Uani 1 1 d . . .
N8 N 1.42362(13) 0.39443(14) -0.13791(13) 0.0295(5) Uani 1 1 d . . .
N9 N 1.07751(13) 0.47278(13) -0.02969(12) 0.0244(4) Uani 1 1 d . . .
N10 N 0.97369(13) 0.41908(14) -0.14673(12) 0.0244(4) Uani 1 1 d . . .
N11 N 1.06104(14) 0.75704(13) -0.03764(13) 0.0293(5) Uani 1 1 d . . .
N12 N 0.96503(15) 0.70545(14) -0.13747(13) 0.0300(5) Uani 1 1 d . . .
O1 O 0.00443(17) 0.33760(17) 0.4122(2) 0.0635(6) Uani 1 1 d . . .
O2 O 0.82764(13) 0.66650(15) -0.25437(15) 0.0434(5) Uani 1 1 d . . .
O3 O 1.15757(16) 0.84708(15) 0.09030(16) 0.0469(5) Uani 1 1 d . . .
O4 O 1.51373(15) 0.49101(16) -0.26522(16) 0.0484(5) Uani 1 1 d D . .
O5 O 0.92569(17) 0.16887(18) 0.15842(15) 0.0598(7) Uani 1 1 d . . .
O6 O 0.83555(18) 0.25906(17) 0.66607(16) 0.0612(7) Uani 1 1 d . . .
Fe1 Fe 1.02526(2) 0.35859(2) -0.08778(3) 0.02211(9) Uani 1 1 d . . .
H4H H 1.485(3) 0.462(3) -0.224(3) 0.079(14) Uiso 1 1 d . . .
H3H H 1.139(2) 0.825(2) 0.051(2) 0.034(9) Uiso 1 1 d . . .
H2H H 0.874(3) 0.684(3) -0.217(3) 0.076(14) Uiso 1 1 d . . .
H2HB H 0.852(3) 0.648(3) -0.294(3) 0.079(14) Uiso 1 1 d . . .
H4HB H 1.485(4) 0.464(4) -0.301(3) 0.14(3) Uiso 1 1 d D . .
H3HB H 1.126(5) 0.813(5) 0.132(4) 0.14(3) Uiso 1 1 d . . .


_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
C1 N1 1.333(3) . ?
C1 C2 1.402(3) . ?
C2 C3 1.380(4) . ?
C3 C4 1.399(4) . ?
C4 C5 1.407(3) . ?
C4 C11 1.429(3) . ?
C5 N1 1.370(3) . ?
C5 C6 1.432(3) . ?
C6 N2 1.364(3) . ?
C6 C7 1.413(3) . ?
C7 C8 1.402(4) . ?
C7 C12 1.427(4) . ?
C8 C9 1.371(4) . ?
C9 C10 1.390(4) . ?
C10 N2 1.340(3) . ?
C11 N3 1.380(3) . ?
C11 C12 1.398(3) . ?
C12 N4 1.378(3) . ?
C13 N4 1.346(4) . ?
C13 N3 1.353(4) . ?
C13 C14 1.469(3) . ?
C14 C15 1.388(5) . ?
C14 C19 1.389(5) . ?
C15 C16 1.387(4) . ?
C16 C17 1.382(7) . ?
C17 C18 1.379(7) . ?
C18 C19 1.388(4) . ?
C20 N5 1.330(3) . ?
C20 C21 1.397(4) . ?
C21 C22 1.370(4) . ?
C22 C23 1.411(4) . ?
C23 C24 1.405(3) . ?
C23 C30 1.419(4) . ?
C24 N5 1.359(3) . ?
C24 C25 1.439(3) . ?
C25 N6 1.366(3) . ?
C25 C26 1.406(3) . ?
C26 C27 1.406(4) . ?
C26 C31 1.433(3) . ?
C27 C28 1.377(4) . ?
C28 C29 1.391(4) . ?
C29 N6 1.335(3) . ?
C30 N7 1.372(3) . ?
C30 C31 1.399(4) . ?
C31 N8 1.365(3) . ?
C32 N7 1.352(4) . ?
C32 N8 1.361(3) . ?
C32 C33 1.472(4) . ?
C33 C38 1.386(4) . ?
C33 C34 1.390(4) . ?
C34 C35 1.388(4) . ?
C35 C36 1.371(5) . ?
C36 C37 1.386(5) . ?
C37 C38 1.386(4) . ?
C39 N9 1.327(3) . ?
C39 C40 1.395(4) . ?
C40 C41 1.378(4) . ?
C41 C42 1.406(4) . ?
C42 C43 1.411(3) . ?
C42 C49 1.428(3) . ?
C43 N9 1.363(3) . ?
C43 C44 1.445(3) . ?
C44 N10 1.359(3) . ?
C44 C45 1.401(3) . ?
C45 C46 1.408(4) . ?
C45 C50 1.422(3) . ?
C46 C47 1.375(4) . ?
C47 C48 1.392(4) . ?
C48 N10 1.337(3) . ?
C49 N11 1.371(3) . ?
C49 C50 1.406(4) . ?
C50 N12 1.364(3) . ?
C51 N12 1.345(4) . ?
C51 N11 1.363(3) . ?
C51 C52 1.471(4) . ?
C52 C53 1.388(4) . ?
C52 C57 1.391(4) . ?
C53 C54 1.387(4) . ?
C54 C55 1.384(5) . ?
C55 C56 1.369(5) . ?
C56 C57 1.384(4) . ?
C61 C62 1.506(7) . ?
C62 O5 1.412(5) . ?
C63 O5 1.426(5) . ?
C63 C64 1.495(7) . ?
C65 C66 1.512(7) . ?
C66 O6 1.410(5) . ?
C67 O6 1.429(5) . ?
C67 C68 1.497(7) . ?
N1 Fe1 1.974(2) . ?
N2 Fe1 1.972(2) . ?
N5 Fe1 1.957(2) . ?
N6 Fe1 1.977(2) . ?
N9 Fe1 1.975(2) . ?
N10 Fe1 1.956(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
N1 C1 C2 122.5(2) . . ?
C3 C2 C1 120.0(2) . . ?
C2 C3 C4 118.7(2) . . ?
C3 C4 C5 118.4(2) . . ?
C3 C4 C11 126.1(2) . . ?
C5 C4 C11 115.5(2) . . ?
N1 C5 C4 122.4(2) . . ?
N1 C5 C6 115.3(2) . . ?
C4 C5 C6 122.3(2) . . ?
N2 C6 C7 122.7(2) . . ?
N2 C6 C5 115.6(2) . . ?
C7 C6 C5 121.8(2) . . ?
C8 C7 C6 117.9(2) . . ?
C8 C7 C12 126.5(2) . . ?
C6 C7 C12 115.6(2) . . ?
C9 C8 C7 118.7(2) . . ?
C8 C9 C10 120.5(2) . . ?
N2 C10 C9 122.6(2) . . ?
N3 C11 C12 108.2(2) . . ?
N3 C11 C4 129.4(2) . . ?
C12 C11 C4 122.4(2) . . ?
N4 C12 C11 108.1(2) . . ?
N4 C12 C7 129.5(2) . . ?
C11 C12 C7 122.4(2) . . ?
N4 C13 N3 113.4(2) . . ?
N4 C13 C14 123.4(3) . . ?
N3 C13 C14 123.1(3) . . ?
C15 C14 C19 119.0(3) . . ?
C15 C14 C13 120.6(3) . . ?
C19 C14 C13 120.4(3) . . ?
C14 C15 C16 120.3(4) . . ?
C17 C16 C15 120.5(4) . . ?
C18 C17 C16 119.3(3) . . ?
C17 C18 C19 120.6(4) . . ?
C18 C19 C14 120.3(4) . . ?
N5 C20 C21 122.6(2) . . ?
C22 C21 C20 119.5(2) . . ?
C21 C22 C23 119.6(2) . . ?
C24 C23 C22 116.9(2) . . ?
C24 C23 C30 116.5(2) . . ?
C22 C23 C30 126.6(2) . . ?
N5 C24 C23 123.1(2) . . ?
N5 C24 C25 115.4(2) . . ?
C23 C24 C25 121.5(2) . . ?
N6 C25 C26 123.4(2) . . ?
N6 C25 C24 115.0(2) . . ?
C26 C25 C24 121.5(2) . . ?
C27 C26 C25 116.9(2) . . ?
C27 C26 C31 126.6(2) . . ?
C25 C26 C31 116.5(2) . . ?
C28 C27 C26 119.4(2) . . ?
C27 C28 C29 120.2(2) . . ?
N6 C29 C28 122.2(2) . . ?
N7 C30 C31 109.2(2) . . ?
N7 C30 C23 128.3(2) . . ?
C31 C30 C23 122.5(2) . . ?
N8 C31 C30 108.7(2) . . ?
N8 C31 C26 129.8(2) . . ?
C30 C31 C26 121.4(2) . . ?
N7 C32 N8 114.9(2) . . ?
N7 C32 C33 122.7(2) . . ?
N8 C32 C33 122.3(3) . . ?
C38 C33 C34 118.4(3) . . ?
C38 C33 C32 121.5(3) . . ?
C34 C33 C32 120.2(3) . . ?
C35 C34 C33 121.2(3) . . ?
C36 C35 C34 119.9(3) . . ?
C35 C36 C37 119.8(3) . . ?
C38 C37 C36 120.3(3) . . ?
C33 C38 C37 120.5(3) . . ?
N9 C39 C40 122.7(2) . . ?
C41 C40 C39 119.9(2) . . ?
C40 C41 C42 119.4(2) . . ?
C41 C42 C43 116.5(2) . . ?
C41 C42 C49 127.0(2) . . ?
C43 C42 C49 116.5(2) . . ?
N9 C43 C42 123.8(2) . . ?
N9 C43 C44 115.0(2) . . ?
C42 C43 C44 121.1(2) . . ?
N10 C44 C45 123.2(2) . . ?
N10 C44 C43 115.1(2) . . ?
C45 C44 C43 121.7(2) . . ?
C44 C45 C46 117.2(2) . . ?
C44 C45 C50 117.0(2) . . ?
C46 C45 C50 125.9(2) . . ?
C47 C46 C45 119.5(2) . . ?
C46 C47 C48 119.6(2) . . ?
N10 C48 C47 122.5(2) . . ?
N11 C49 C50 108.1(2) . . ?
N11 C49 C42 129.7(2) . . ?
C50 C49 C42 122.0(2) . . ?
N12 C50 C49 109.2(2) . . ?
N12 C50 C45 129.1(2) . . ?
C49 C50 C45 121.6(2) . . ?
N12 C51 N11 114.9(2) . . ?
N12 C51 C52 122.9(2) . . ?
N11 C51 C52 122.1(3) . . ?
C53 C52 C57 118.4(3) . . ?
C53 C52 C51 121.5(3) . . ?
C57 C52 C51 120.1(3) . . ?
C54 C53 C52 120.3(3) . . ?
C55 C54 C53 120.6(3) . . ?
C56 C55 C54 119.4(3) . . ?
C55 C56 C57 120.5(3) . . ?
C56 C57 C52 120.8(3) . . ?
O5 C62 C61 110.0(3) . . ?
O5 C63 C64 110.4(3) . . ?
O6 C66 C65 110.0(3) . . ?
O6 C67 C68 110.1(4) . . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 128.82(16) . . ?
C5 N1 Fe1 113.11(17) . . ?
C10 N2 C6 117.7(2) . . ?
C10 N2 Fe1 129.04(17) . . ?
C6 N2 Fe1 113.28(17) . . ?
C13 N3 C11 105.0(2) . . ?
C13 N4 C12 105.3(2) . . ?
C20 N5 C24 118.2(2) . . ?
C20 N5 Fe1 127.98(17) . . ?
C24 N5 Fe1 113.76(17) . . ?
C29 N6 C25 117.9(2) . . ?
C29 N6 Fe1 129.06(16) . . ?
C25 N6 Fe1 113.03(17) . . ?
C32 N7 C30 103.4(2) . . ?
C32 N8 C31 103.8(2) . . ?
C39 N9 C43 117.6(2) . . ?
C39 N9 Fe1 129.22(16) . . ?
C43 N9 Fe1 113.16(17) . . ?
C48 N10 C44 118.1(2) . . ?
C48 N10 Fe1 127.98(16) . . ?
C44 N10 Fe1 113.90(17) . . ?
C51 N11 C49 103.8(2) . . ?
C51 N12 C50 103.9(2) . . ?
C62 O5 C63 114.3(3) . . ?
C66 O6 C67 114.0(3) . . ?
N10 Fe1 N5 175.63(9) . . ?
N10 Fe1 N2 93.84(9) . . ?
N5 Fe1 N2 89.46(9) . . ?
N10 Fe1 N1 89.50(9) . . ?
N5 Fe1 N1 93.76(9) . . ?
N2 Fe1 N1 82.71(8) . . ?
N10 Fe1 N9 82.76(9) . . ?
N5 Fe1 N9 94.10(9) . . ?
N2 Fe1 N9 175.42(9) . . ?
N1 Fe1 N9 94.16(9) . . ?
N10 Fe1 N6 94.14(9) . . ?
N5 Fe1 N6 82.75(9) . . ?
N2 Fe1 N6 94.23(9) . . ?
N1 Fe1 N6 175.40(9) . . ?
N9 Fe1 N6 89.10(8) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        73.55
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.050

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.055 0.461 0.188 24 2 ' '
2 0.165 0.666 0.744 66 5 ' '
3 0.129 0.280 0.637 24 2 ' '
4 0.151 0.871 0.303 25 2 ' '
5 0.334 0.500 0.078 66 5 ' '
6 0.500 0.835 0.411 66 5 ' '
7 0.516 0.055 0.855 24 2 ' '
8 0.539 0.484 0.522 24 2 ' '
9 0.720 0.849 -0.030 24 2 ' '
_platon_squeeze_details          
;
The unit cell contains disordered solvent molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 344 A3 containing about 28 electrons which corresponds to approximately 1 water molecule per formula unit. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1835925'
_audit_update_record             
;
2018-04-10 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H33 N12 Co, H9 O4, C8 H20 O2, H4 O2'
_chemical_formula_sum            'C65 H66 Co N12 O8'
_chemical_formula_weight         1202.23

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R32

loop_
_symmetry_equiv_pos_as_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                   17.0790(13)
_cell_length_b                   17.0790(13)
_cell_length_c                   17.9429(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4532.6(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    2126
_cell_measurement_theta_min      3.8130
_cell_measurement_theta_max      70.0240

_exptl_crystal_description       prismatic
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1893
_exptl_absorpt_coefficient_mu    2.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.543
_oxdiff_exptl_absorpt_empirical_full_max 2.606
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8032
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.87
_diffrn_reflns_theta_max         73.61
_reflns_number_total             2024
_reflns_number_gt                1613
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0805P)²+0.2057P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         2024
_refine_ls_number_parameters     117
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1468
_refine_ls_wR_factor_gt          0.1330
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9661(3) 0.8592(3) 0.88085(19) 0.0791(9) Uani 1 1 d . . .
H1 H 1.0232 0.8994 0.8623 0.095 Uiso 1 1 calc R . .
C2 C 0.9148(3) 0.7763(3) 0.8462(2) 0.0842(10) Uani 1 1 d . . .
H2 H 0.9374 0.7621 0.8044 0.101 Uiso 1 1 calc R . .
C3 C 0.8317(3) 0.7156(3) 0.8730(2) 0.0867(10) Uani 1 1 d . . .
H3 H 0.7975 0.6598 0.8498 0.104 Uiso 1 1 calc R . .
C4 C 0.7982(3) 0.7378(3) 0.9353(2) 0.0826(9) Uani 1 1 d . . .
C5 C 0.8528(2) 0.8236(3) 0.96801(19) 0.0741(8) Uani 1 1 d . . .
C6 C 0.7113(3) 0.6816(3) 0.9694(2) 0.0898(11) Uani 1 1 d . . .
C7 C 0.5777(4) 0.5777(4) 1.0000 0.0990(17) Uani 1 2 d S . .
C8 C 0.4921(4) 0.4921(4) 1.0000 0.0971(15) Uani 1 2 d S . .
C9 C 0.4822(4) 0.4183(3) 0.9633(3) 0.1148(16) Uani 1 1 d . . .
H9 H 0.5313 0.4215 0.9381 0.138 Uiso 1 1 calc R . .
C10 C 0.3997(5) 0.3377(4) 0.9626(4) 0.140(2) Uani 1 1 d . . .
H10 H 0.3939 0.2887 0.9354 0.168 Uiso 1 1 calc R . .
C11 C 0.3299(5) 0.3299(5) 1.0000 0.145(4) Uani 1 2 d S . .
H11 H 0.2755 0.2755 1.0000 0.174 Uiso 1 2 calc SR . .
N1 N 0.9352(2) 0.88297(18) 0.94088(14) 0.0731(7) Uani 1 1 d . . .
N2 N 0.6451(3) 0.5959(2) 0.9509(2) 0.0930(10) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.8333 0.0974(16) Uani 1 6 d SD . .
O2 O 0.6667 0.4967(2) 0.8333 0.1000(12) Uani 1 2 d S . .
Co1 Co 1.0000 1.0000 1.0000 0.0650(3) Uani 1 6 d S . .
H1H H 0.6667 0.3923(12) 0.8333 0.27(7) Uiso 1 2 d SD . .


_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
C1 N1 1.348(5) . ?
C1 C2 1.384(6) . ?
C2 C3 1.360(5) . ?
C3 C4 1.393(6) . ?
C4 C5 1.412(5) . ?
C4 C6 1.440(5) . ?
C5 N1 1.348(5) . ?
C5 C5 1.436(7) 6_557 ?
C6 N2 1.370(6) . ?
C6 C6 1.407(8) 6_557 ?
C7 N2 1.357(5) . ?
C7 N2 1.357(5) 6_557 ?
C7 C8 1.461(10) . ?
C8 C9 1.356(6) . ?
C8 C9 1.356(6) 6_557 ?
C9 C10 1.392(7) . ?
C10 C11 1.316(8) . ?
C11 C10 1.316(8) 6_557 ?
N1 Co1 2.033(3) . ?
Co1 N1 2.033(3) 3_675 ?
Co1 N1 2.033(3) 6_557 ?
Co1 N1 2.033(3) 5_767 ?
Co1 N1 2.033(3) 2_765 ?
Co1 N1 2.033(3) 4_677 ?

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 C1 C2 121.6(3) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 119.4(4) . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 C6 125.9(4) . . ?
C5 C4 C6 116.2(4) . . ?
N1 C5 C4 122.0(3) . . ?
N1 C5 C5 116.1(2) . 6_557 ?
C4 C5 C5 121.9(2) . 6_557 ?
N2 C6 C6 108.7(3) . 6_557 ?
N2 C6 C4 129.4(4) . . ?
C6 C6 C4 121.9(2) 6_557 . ?
N2 C7 N2 114.8(6) . 6_557 ?
N2 C7 C8 122.6(3) . . ?
N2 C7 C8 122.6(3) 6_557 . ?
C9 C8 C9 116.3(7) . 6_557 ?
C9 C8 C7 121.8(4) . . ?
C9 C8 C7 121.8(4) 6_557 . ?
C8 C9 C10 121.2(7) . . ?
C11 C10 C9 120.8(7) . . ?
C10 C11 C10 119.5(8) . 6_557 ?
C1 N1 C5 118.7(3) . . ?
C1 N1 Co1 127.6(3) . . ?
C5 N1 Co1 113.7(2) . . ?
C7 N2 C6 103.9(4) . . ?
N1 Co1 N1 89.39(18) 3_675 6_557 ?
N1 Co1 N1 173.9(2) 3_675 5_767 ?
N1 Co1 N1 95.26(9) 6_557 5_767 ?
N1 Co1 N1 95.26(9) 3_675 2_765 ?
N1 Co1 N1 173.9(2) 6_557 2_765 ?
N1 Co1 N1 80.39(18) 5_767 2_765 ?
N1 Co1 N1 95.26(9) 3_675 . ?
N1 Co1 N1 80.39(18) 6_557 . ?
N1 Co1 N1 89.39(18) 5_767 . ?
N1 Co1 N1 95.26(9) 2_765 . ?
N1 Co1 N1 80.39(18) 3_675 4_677 ?
N1 Co1 N1 95.26(9) 6_557 4_677 ?
N1 Co1 N1 95.26(9) 5_767 4_677 ?
N1 Co1 N1 89.39(18) 2_765 4_677 ?
N1 Co1 N1 173.9(2) . 4_677 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        73.61
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.035

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 -0.011 0.167 463 111 ' '
2 -0.006 -0.004 0.833 463 111 ' '
3 -0.018 0.475 0.500 464 111 ' '
_platon_squeeze_details          
;
The unit cell contains disordered diethylether and water molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 1394 A3 containing about 332 electrons which corresponds to approximately 2 molecules of diethylether and 2 water molecules per formula unit. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
# start Validation Reply Form
_vrf_CHEMW03_2                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert origins from the number of solvent molecules 
(2 diethyl ether, 2 water) calculated by using 
SQUEEZE/PLATON procedure and inserted in the 
empirical formula and molecular weight.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_1c
_database_code_depnum_ccdc_archive 'CCDC 1835924'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'H9 O4, C57 H33 N12 Fe, C8 H18 O, C4 H8 O, H2 O'
_chemical_formula_sum            'C69 H70 Fe N12 O7'
_chemical_formula_weight         1235.22

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P31

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   17.0080(15)
_cell_length_b                   17.0080(15)
_cell_length_c                   18.4960(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4633.6(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    1595
_cell_measurement_theta_min      2.9470
_cell_measurement_theta_max      62.5930

_exptl_crystal_description       prismatic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1950
_exptl_absorpt_coefficient_mu    2.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75508
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.780
_oxdiff_exptl_absorpt_empirical_full_max 1.227
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24132
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         73.57
_reflns_number_total             12062
_reflns_number_gt                6655
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0970P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         12062
_refine_ls_number_parameters     687
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0828
_refine_ls_wR_factor_ref         0.2231
_refine_ls_wR_factor_gt          0.1954
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_restrained_S_all      0.938
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5790(4) 0.8734(5) 0.0313(4) 0.0635(18) Uani 1 1 d . . .
H1 H 0.5637 0.9151 0.0492 0.076 Uiso 1 1 calc R . .
C2 C 0.5483(4) 0.7918(5) 0.0669(4) 0.0673(19) Uani 1 1 d . . .
H2 H 0.5128 0.7793 0.1082 0.081 Uiso 1 1 calc R . .
C3 C 0.5698(5) 0.7297(5) 0.0419(4) 0.0680(19) Uani 1 1 d . . .
H3 H 0.5485 0.6748 0.0660 0.082 Uiso 1 1 calc R . .
C4 C 0.6238(4) 0.7481(5) -0.0200(4) 0.0633(17) Uani 1 1 d . . .
C5 C 0.6554(4) 0.8358(5) -0.0543(4) 0.0640(18) Uani 1 1 d . . .
C6 C 0.7113(4) 0.8606(4) -0.1157(3) 0.0536(15) Uani 1 1 d . . .
C7 C 0.7404(4) 0.8057(5) -0.1475(5) 0.073(2) Uani 1 1 d . . .
C8 C 0.7940(4) 0.8365(6) -0.2109(4) 0.075(2) Uani 1 1 d . . .
H8 H 0.8127 0.8010 -0.2355 0.090 Uiso 1 1 calc R . .
C9 C 0.8174(4) 0.9241(6) -0.2346(5) 0.074(2) Uani 1 1 d . . .
H9 H 0.8551 0.9482 -0.2747 0.089 Uiso 1 1 calc R . .
C10 C 0.7872(4) 0.9747(5) -0.2015(3) 0.0611(17) Uani 1 1 d . . .
H10 H 0.8042 1.0314 -0.2208 0.073 Uiso 1 1 calc R . .
C11 C 0.6519(5) 0.6893(6) -0.0519(4) 0.074(2) Uani 1 1 d . . .
C12 C 0.7097(5) 0.7166(6) -0.1147(4) 0.074(2) Uani 1 1 d . . .
C13 C 0.6741(6) 0.5805(6) -0.0856(5) 0.085(3) Uani 1 1 d . . .
C14 C 0.6644(7) 0.4918(7) -0.0892(6) 0.092(3) Uani 1 1 d . . .
C15 C 0.6012(8) 0.4198(7) -0.0497(6) 0.115(4) Uani 1 1 d . . .
H15 H 0.5610 0.4279 -0.0209 0.138 Uiso 1 1 calc R . .
C16 C 0.5948(11) 0.3356(8) -0.0507(8) 0.140(5) Uani 1 1 d . . .
H16 H 0.5527 0.2900 -0.0208 0.168 Uiso 1 1 calc R . .
C17 C 0.6457(9) 0.3182(9) -0.0918(7) 0.124(5) Uani 1 1 d . . .
H17 H 0.6386 0.2605 -0.0944 0.148 Uiso 1 1 calc R . .
C18 C 0.7101(10) 0.3887(9) -0.1314(7) 0.118(4) Uani 1 1 d . . .
H18 H 0.7492 0.3782 -0.1596 0.142 Uiso 1 1 calc R . .
C19 C 0.7207(7) 0.4749(7) -0.1320(6) 0.100(3) Uani 1 1 d . . .
H19 H 0.7648 0.5205 -0.1608 0.120 Uiso 1 1 calc R . .
C20 C 0.8178(4) 1.0393(5) 0.0306(4) 0.069(2) Uani 1 1 d . . .
H20 H 0.7762 0.9824 0.0487 0.082 Uiso 1 1 calc R . .
C21 C 0.9008(4) 1.0919(5) 0.0658(4) 0.066(2) Uani 1 1 d . . .
H21 H 0.9147 1.0694 0.1067 0.079 Uiso 1 1 calc R . .
C22 C 0.9621(4) 1.1768(5) 0.0400(4) 0.0653(18) Uani 1 1 d . . .
H22 H 1.0168 1.2120 0.0640 0.078 Uiso 1 1 calc R . .
C23 C 0.9425(3) 1.2099(5) -0.0215(4) 0.0593(17) Uani 1 1 d . . .
C24 C 0.8564(3) 1.1544(4) -0.0538(4) 0.0565(16) Uani 1 1 d . . .
C25 C 0.8288(3) 1.1805(4) -0.1178(4) 0.0556(16) Uani 1 1 d . . .
C26 C 0.8858(4) 1.2697(4) -0.1521(4) 0.0607(17) Uani 1 1 d . . .
C27 C 0.8494(4) 1.2863(5) -0.2139(4) 0.0596(16) Uani 1 1 d . . .
H27 H 0.8831 1.3405 -0.2389 0.072 Uiso 1 1 calc R . .
C28 C 0.7663(4) 1.2249(5) -0.2377(4) 0.0623(18) Uani 1 1 d . . .
H28 H 0.7425 1.2377 -0.2783 0.075 Uiso 1 1 calc R . .
C29 C 0.7151(4) 1.1418(5) -0.2020(4) 0.0662(18) Uani 1 1 d . . .
H29 H 0.6584 1.1006 -0.2207 0.079 Uiso 1 1 calc R . .
C30 C 0.9971(4) 1.2985(5) -0.0559(4) 0.0646(19) Uani 1 1 d . . .
C31 C 0.9696(4) 1.3242(5) -0.1175(4) 0.0619(18) Uani 1 1 d . . .
C32 C 1.1019(4) 1.4321(5) -0.0838(4) 0.0619(18) Uani 1 1 d . . .
C33 C 1.1851(5) 1.5189(5) -0.0837(5) 0.0651(18) Uani 1 1 d . . .
C34 C 1.2549(4) 1.5336(5) -0.0347(4) 0.073(2) Uani 1 1 d . . .
H34 H 1.2478 1.4876 -0.0034 0.087 Uiso 1 1 calc R . .
C35 C 1.3341(6) 1.6174(7) -0.0337(5) 0.086(3) Uani 1 1 d . . .
H35 H 1.3803 1.6281 -0.0014 0.103 Uiso 1 1 calc R . .
C36 C 1.3442(7) 1.6852(7) -0.0810(7) 0.115(4) Uani 1 1 d . . .
H36 H 1.3965 1.7419 -0.0794 0.138 Uiso 1 1 calc R . .
C37 C 1.2793(7) 1.6693(6) -0.1287(6) 0.112(4) Uani 1 1 d . . .
H37 H 1.2882 1.7145 -0.1615 0.134 Uiso 1 1 calc R . .
C38 C 1.1990(6) 1.5869(6) -0.1305(6) 0.097(3) Uani 1 1 d . . .
H38 H 1.1541 1.5778 -0.1638 0.117 Uiso 1 1 calc R . .
C39 C 0.5469(4) 0.9038(5) -0.2012(4) 0.071(2) Uani 1 1 d . . .
H39 H 0.5876 0.8873 -0.2192 0.085 Uiso 1 1 calc R . .
C40 C 0.4638(5) 0.8716(6) -0.2367(5) 0.077(2) Uani 1 1 d . . .
H40 H 0.4503 0.8355 -0.2777 0.092 Uiso 1 1 calc R . .
C41 C 0.4016(4) 0.8947(5) -0.2092(4) 0.070(2) Uani 1 1 d . . .
H41 H 0.3456 0.8734 -0.2316 0.084 Uiso 1 1 calc R . .
C42 C 0.4229(4) 0.9485(6) -0.1494(4) 0.071(2) Uani 1 1 d . . .
C43 C 0.5102(4) 0.9790(5) -0.1172(4) 0.0599(17) Uani 1 1 d . . .
C44 C 0.5372(3) 1.0374(5) -0.0547(4) 0.0585(17) Uani 1 1 d . . .
C45 C 0.4840(4) 1.0666(6) -0.0236(4) 0.074(2) Uani 1 1 d . . .
C46 C 0.5140(4) 1.1217(5) 0.0381(5) 0.072(2) Uani 1 1 d . . .
H46 H 0.4798 1.1437 0.0603 0.086 Uiso 1 1 calc R . .
C47 C 0.5993(4) 1.1412(5) 0.0639(4) 0.0675(19) Uani 1 1 d . . .
H47 H 0.6218 1.1752 0.1060 0.081 Uiso 1 1 calc R . .
C48 C 0.6498(4) 1.1120(5) 0.0293(4) 0.070(2) Uani 1 1 d . . .
H48 H 0.7074 1.1298 0.0473 0.084 Uiso 1 1 calc R . .
C49 C 0.3671(4) 0.9778(6) -0.1167(4) 0.069(2) Uani 1 1 d . . .
C50 C 0.3960(5) 1.0376(7) -0.0569(5) 0.085(3) Uani 1 1 d . . .
C51 C 0.2590(5) 1.0027(6) -0.0861(5) 0.076(2) Uani 1 1 d . . .
C52 C 0.1707(5) 0.9968(7) -0.0848(5) 0.077(2) Uani 1 1 d . . .
C53 C 0.0985(5) 0.9354(7) -0.1186(5) 0.094(3) Uani 1 1 d . . .
H53 H 0.1041 0.8922 -0.1454 0.112 Uiso 1 1 calc R . .
C54 C 0.0143(7) 0.9297(11) -0.1175(7) 0.140(5) Uani 1 1 d . . .
H54 H -0.0343 0.8834 -0.1424 0.168 Uiso 1 1 calc R . .
C55 C 0.0027(10) 0.9945(13) -0.0785(8) 0.161(7) Uani 1 1 d . . .
H55 H -0.0531 0.9922 -0.0764 0.193 Uiso 1 1 calc R . .
C56 C 0.0775(8) 1.0604(11) -0.0441(7) 0.136(5) Uani 1 1 d . . .
H56 H 0.0722 1.1035 -0.0169 0.163 Uiso 1 1 calc R . .
C57 C 0.1621(7) 1.0655(9) -0.0485(7) 0.115(4) Uani 1 1 d . . .
H57 H 0.2129 1.1141 -0.0275 0.138 Uiso 1 1 calc R . .
N1 N 0.6306(3) 0.8942(4) -0.0288(3) 0.0545(14) Uani 1 1 d . . .
N2 N 0.7332(3) 0.9480(4) -0.1415(3) 0.0616(16) Uani 1 1 d . . .
N3 N 0.6306(4) 0.6043(5) -0.0361(4) 0.082(2) Uani 1 1 d . . .
N4 N 0.7216(4) 0.6474(5) -0.1334(4) 0.083(2) Uani 1 1 d . . .
N5 N 0.7981(3) 1.0703(4) -0.0282(3) 0.0616(15) Uani 1 1 d . . .
N6 N 0.7429(3) 1.1185(4) -0.1431(3) 0.0557(14) Uani 1 1 d . . .
N7 N 1.0814(3) 1.3661(4) -0.0340(3) 0.0608(15) Uani 1 1 d . . .
N8 N 1.0353(3) 1.4092(4) -0.1340(3) 0.0625(15) Uani 1 1 d . . .
N9 N 0.5710(3) 0.9569(4) -0.1427(3) 0.0604(15) Uani 1 1 d . . .
N10 N 0.6219(3) 1.0587(4) -0.0297(3) 0.0593(16) Uani 1 1 d . . .
N11 N 0.2798(4) 0.9567(5) -0.1345(4) 0.088(2) Uani 1 1 d . . .
N12 N 0.3273(4) 1.0545(5) -0.0375(4) 0.085(2) Uani 1 1 d . . .
Fe1 Fe 0.68349(5) 1.00797(12) -0.08579(6) 0.0559(3) Uani 1 1 d . . .
O1 O 0.3414(5) 0.1688(4) 0.0773(4) 0.0968(17) Uani 1 1 d . . .
O2 O 0.6698(4) 0.0016(5) 0.4166(5) 0.1037(16) Uani 1 1 d . . .
O3 O 0.0092(4) 0.5059(4) 0.7449(4) 0.0931(17) Uani 1 1 d . . .
O4 O 1.1736(3) 1.3489(4) 0.0881(3) 0.0813(15) Uani 1 1 d . . .
C1S C 0.5224(10) 0.1611(10) 0.7336(7) 0.148(5) Uiso 1 1 d . . .
H1S1 H 0.4685 0.1660 0.7354 0.222 Uiso 1 1 calc R . .
H1S2 H 0.5749 0.2208 0.7325 0.222 Uiso 1 1 calc R . .
H1S3 H 0.5248 0.1293 0.7756 0.222 Uiso 1 1 calc R . .
C2S C 0.5205(12) 0.1103(12) 0.6672(11) 0.200(7) Uiso 1 1 d . . .
H2S1 H 0.4653 0.0516 0.6670 0.240 Uiso 1 1 calc R . .
H2S2 H 0.5195 0.1435 0.6248 0.240 Uiso 1 1 calc R . .
O1S O 0.5998(6) 0.0968(6) 0.6627(5) 0.141(3) Uiso 1 1 d . . .
C3S C 0.6101(10) 0.0394(10) 0.6062(8) 0.157(5) Uiso 1 1 d . . .
H3S1 H 0.6148 0.0661 0.5589 0.188 Uiso 1 1 calc R . .
H3S2 H 0.5568 -0.0208 0.6063 0.188 Uiso 1 1 calc R . .
C4S C 0.6965(10) 0.0319(10) 0.6210(9) 0.160(6) Uiso 1 1 d . . .
H4S1 H 0.7036 -0.0027 0.5832 0.240 Uiso 1 1 calc R . .
H4S2 H 0.6902 0.0022 0.6666 0.240 Uiso 1 1 calc R . .
H4S3 H 0.7490 0.0916 0.6224 0.240 Uiso 1 1 calc R . .


_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
C1 N1 1.350(9) . ?
C1 C2 1.381(10) . ?
C2 C3 1.358(11) . ?
C3 C4 1.403(10) . ?
C4 C11 1.433(11) . ?
C4 C5 1.454(10) . ?
C5 N1 1.344(9) . ?
C5 C6 1.403(9) . ?
C6 C7 1.388(10) . ?
C6 N2 1.422(9) . ?
C7 C8 1.416(11) . ?
C7 C12 1.465(11) . ?
C8 C9 1.406(11) . ?
C9 C10 1.349(11) . ?
C10 N2 1.365(9) . ?
C11 N3 1.336(11) . ?
C11 C12 1.440(11) . ?
C12 N4 1.335(11) . ?
C13 N4 1.345(12) . ?
C13 N3 1.361(12) . ?
C13 C14 1.435(13) . ?
C14 C15 1.369(15) . ?
C14 C19 1.378(15) . ?
C15 C16 1.381(15) . ?
C16 C17 1.292(18) . ?
C17 C18 1.363(17) . ?
C18 C19 1.386(15) . ?
C20 N5 1.323(9) . ?
C20 C21 1.397(8) . ?
C21 C22 1.377(9) . ?
C22 C23 1.382(10) . ?
C23 C24 1.418(7) . ?
C23 C30 1.463(10) . ?
C24 N5 1.355(9) . ?
C24 C25 1.422(9) . ?
C25 N6 1.388(7) . ?
C25 C26 1.475(9) . ?
C26 C27 1.394(10) . ?
C26 C31 1.406(8) . ?
C27 C28 1.344(8) . ?
C28 C29 1.400(10) . ?
C29 N6 1.324(9) . ?
C30 N7 1.375(7) . ?
C30 C31 1.382(10) . ?
C31 N8 1.347(9) . ?
C32 N7 1.356(10) . ?
C32 N8 1.363(9) . ?
C32 C33 1.447(9) . ?
C33 C38 1.368(13) . ?
C33 C34 1.413(11) . ?
C34 C35 1.388(11) . ?
C35 C36 1.388(15) . ?
C36 C37 1.330(16) . ?
C37 C38 1.385(11) . ?
C39 N9 1.336(9) . ?
C39 C40 1.398(9) . ?
C40 C41 1.397(11) . ?
C41 C42 1.364(11) . ?
C42 C49 1.410(11) . ?
C42 C43 1.436(7) . ?
C43 N9 1.349(9) . ?
C43 C44 1.441(10) . ?
C44 C45 1.358(10) . ?
C44 N10 1.377(7) . ?
C45 C46 1.401(11) . ?
C45 C50 1.458(9) . ?
C46 C47 1.401(9) . ?
C47 C48 1.350(11) . ?
C48 N10 1.344(10) . ?
C49 N11 1.381(8) . ?
C49 C50 1.414(11) . ?
C50 N12 1.383(10) . ?
C51 N11 1.346(11) . ?
C51 N12 1.382(11) . ?
C51 C52 1.455(10) . ?
C52 C53 1.306(13) . ?
C52 C57 1.416(15) . ?
C53 C54 1.386(12) . ?
C54 C55 1.41(2) . ?
C55 C56 1.36(2) . ?
C56 C57 1.402(13) . ?
N1 Fe1 1.980(6) . ?
N2 Fe1 1.919(7) . ?
N5 Fe1 1.998(5) . ?
N6 Fe1 1.944(6) . ?
N9 Fe1 1.965(5) . ?
N10 Fe1 1.955(6) . ?
C1S C2S 1.495(19) . ?
C2S O1S 1.479(18) . ?
O1S C3S 1.498(15) . ?
C3S C4S 1.563(18) . ?

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 C1 C2 121.7(7) . . ?
C3 C2 C1 120.4(7) . . ?
C2 C3 C4 120.3(7) . . ?
C3 C4 C11 126.2(7) . . ?
C3 C4 C5 116.7(7) . . ?
C11 C4 C5 117.1(7) . . ?
N1 C5 C6 118.5(6) . . ?
N1 C5 C4 120.9(6) . . ?
C6 C5 C4 120.6(7) . . ?
C7 C6 C5 123.8(7) . . ?
C7 C6 N2 124.4(6) . . ?
C5 C6 N2 111.7(6) . . ?
C6 C7 C8 118.8(7) . . ?
C6 C7 C12 117.2(7) . . ?
C8 C7 C12 123.9(8) . . ?
C9 C8 C7 116.1(8) . . ?
C10 C9 C8 122.5(8) . . ?
C9 C10 N2 124.4(7) . . ?
N3 C11 C4 131.3(8) . . ?
N3 C11 C12 107.3(8) . . ?
C4 C11 C12 121.3(8) . . ?
N4 C12 C11 107.7(8) . . ?
N4 C12 C7 132.2(8) . . ?
C11 C12 C7 120.0(8) . . ?
N4 C13 N3 112.1(8) . . ?
N4 C13 C14 124.3(10) . . ?
N3 C13 C14 123.4(9) . . ?
C15 C14 C19 115.9(11) . . ?
C15 C14 C13 122.8(11) . . ?
C19 C14 C13 121.2(10) . . ?
C14 C15 C16 122.7(13) . . ?
C17 C16 C15 122.0(14) . . ?
C16 C17 C18 116.8(12) . . ?
C17 C18 C19 123.8(12) . . ?
C14 C19 C18 118.6(11) . . ?
N5 C20 C21 120.3(7) . . ?
C22 C21 C20 120.2(7) . . ?
C21 C22 C23 120.1(6) . . ?
C22 C23 C24 117.1(6) . . ?
C22 C23 C30 128.3(5) . . ?
C24 C23 C30 114.5(6) . . ?
N5 C24 C23 121.5(6) . . ?
N5 C24 C25 116.0(5) . . ?
C23 C24 C25 122.4(6) . . ?
N6 C25 C24 115.5(5) . . ?
N6 C25 C26 122.5(6) . . ?
C24 C25 C26 121.9(5) . . ?
C27 C26 C31 130.2(6) . . ?
C27 C26 C25 115.5(5) . . ?
C31 C26 C25 114.3(6) . . ?
C28 C27 C26 120.8(6) . . ?
C27 C28 C29 120.8(6) . . ?
N6 C29 C28 123.7(6) . . ?
N7 C30 C31 110.8(6) . . ?
N7 C30 C23 126.2(7) . . ?
C31 C30 C23 122.9(5) . . ?
N8 C31 C30 107.2(6) . . ?
N8 C31 C26 128.9(7) . . ?
C30 C31 C26 123.9(6) . . ?
N7 C32 N8 113.2(5) . . ?
N7 C32 C33 124.1(6) . . ?
N8 C32 C33 122.8(7) . . ?
C38 C33 C34 118.9(7) . . ?
C38 C33 C32 122.0(8) . . ?
C34 C33 C32 119.1(8) . . ?
C35 C34 C33 119.2(8) . . ?
C36 C35 C34 119.9(8) . . ?
C37 C36 C35 120.3(8) . . ?
C36 C37 C38 121.4(11) . . ?
C33 C38 C37 120.3(10) . . ?
N9 C39 C40 123.6(7) . . ?
C41 C40 C39 118.6(7) . . ?
C42 C41 C40 120.0(6) . . ?
C41 C42 C49 125.8(6) . . ?
C41 C42 C43 117.3(7) . . ?
C49 C42 C43 116.9(7) . . ?
N9 C43 C42 123.5(7) . . ?
N9 C43 C44 116.6(5) . . ?
C42 C43 C44 119.8(6) . . ?
C45 C44 N10 124.2(7) . . ?
C45 C44 C43 123.4(5) . . ?
N10 C44 C43 112.4(6) . . ?
C44 C45 C46 120.2(6) . . ?
C44 C45 C50 117.1(7) . . ?
C46 C45 C50 122.7(7) . . ?
C47 C46 C45 115.1(7) . . ?
C48 C47 C46 121.7(7) . . ?
N10 C48 C47 123.9(6) . . ?
N11 C49 C42 129.2(7) . . ?
N11 C49 C50 108.4(7) . . ?
C42 C49 C50 122.4(6) . . ?
N12 C50 C49 109.0(6) . . ?
N12 C50 C45 130.6(8) . . ?
C49 C50 C45 120.3(7) . . ?
N11 C51 N12 115.0(6) . . ?
N11 C51 C52 122.2(8) . . ?
N12 C51 C52 122.8(8) . . ?
C53 C52 C57 116.3(8) . . ?
C53 C52 C51 124.9(10) . . ?
C57 C52 C51 118.7(9) . . ?
C52 C53 C54 125.0(13) . . ?
C53 C54 C55 119.8(13) . . ?
C56 C55 C54 116.3(10) . . ?
C55 C56 C57 122.1(14) . . ?
C56 C57 C52 120.2(12) . . ?
C5 N1 C1 119.9(6) . . ?
C5 N1 Fe1 112.3(5) . . ?
C1 N1 Fe1 127.8(5) . . ?
C10 N2 C6 113.7(6) . . ?
C10 N2 Fe1 131.4(5) . . ?
C6 N2 Fe1 114.8(5) . . ?
C11 N3 C13 106.3(7) . . ?
C12 N4 C13 106.5(8) . . ?
C20 N5 C24 120.7(5) . . ?
C20 N5 Fe1 127.0(4) . . ?
C24 N5 Fe1 112.2(5) . . ?
C29 N6 C25 116.6(6) . . ?
C29 N6 Fe1 130.3(4) . . ?
C25 N6 Fe1 113.0(4) . . ?
C32 N7 C30 102.7(6) . . ?
C31 N8 C32 106.1(6) . . ?
C39 N9 C43 117.0(5) . . ?
C39 N9 Fe1 129.4(5) . . ?
C43 N9 Fe1 113.7(5) . . ?
C48 N10 C44 114.9(6) . . ?
C48 N10 Fe1 129.9(4) . . ?
C44 N10 Fe1 115.3(5) . . ?
C51 N11 C49 104.5(7) . . ?
C51 N12 C50 103.1(7) . . ?
N2 Fe1 N6 93.9(3) . . ?
N2 Fe1 N10 174.7(2) . . ?
N6 Fe1 N10 89.8(3) . . ?
N2 Fe1 N9 93.9(2) . . ?
N6 Fe1 N9 93.2(2) . . ?
N10 Fe1 N9 82.0(2) . . ?
N2 Fe1 N1 82.6(3) . . ?
N6 Fe1 N1 175.9(2) . . ?
N10 Fe1 N1 93.8(2) . . ?
N9 Fe1 N1 89.3(2) . . ?
N2 Fe1 N5 89.8(2) . . ?
N6 Fe1 N5 83.1(2) . . ?
N10 Fe1 N5 94.5(2) . . ?
N9 Fe1 N5 175.0(3) . . ?
N1 Fe1 N5 94.6(2) . . ?
O1S C2S C1S 112.2(14) . . ?
C2S O1S C3S 123.5(12) . . ?
O1S C3S C4S 110.6(12) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        73.57
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.053

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.327 0.421 0.798 315 89 ' '
2 0.094 0.673 0.465 316 88 ' '
3 0.579 0.906 1.131 316 89 ' '
_platon_squeeze_details          
;
The unit cell contains disordered solvent molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 952 A3 containing about 266 electrons which corresponds to approximately 1 dibutyl ether and 1 water molecules. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
# start Validation Reply Form
_vrf_CHEMW03_1c                  
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert origins from the number of solvent molecules (1 dibutyl ether, 1 water) calculated by using SQUEEZE/PLATON procedure and inserted in the empirical formula and molecular weight.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1835926'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Fe C60 H30 F9 N12, C8 H24 O4, H14 O7'
_chemical_formula_sum            'C68 H68 F9 Fe N12 O11'
_chemical_formula_weight         1456.19

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'

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

_cell_length_a                   17.7212(4)
_cell_length_b                   18.6855(6)
_cell_length_c                   20.2478(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6704.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    8173
_cell_measurement_theta_min      3.4230
_cell_measurement_theta_max      71.8810

_exptl_crystal_description       prismatic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3020
_exptl_absorpt_coefficient_mu    2.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.789
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26628
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         73.41
_reflns_number_total             12452
_reflns_number_gt                10164
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1274P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(4)
_refine_ls_number_reflns         12452
_refine_ls_number_parameters     767
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1839
_refine_ls_wR_factor_gt          0.1705
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.11176(3) 0.84780(3) 0.79900(3) 0.04207(14) Uani 1 1 d . . .
C1 C 0.9776(2) 0.7625(2) 0.7549(2) 0.0486(8) Uani 1 1 d . . .
H1 H 1.0104 0.7337 0.7308 0.058 Uiso 1 1 calc R . .
C2 C 0.9022(3) 0.7469(3) 0.7546(2) 0.0572(10) Uani 1 1 d . . .
H2 H 0.8849 0.7076 0.7307 0.069 Uiso 1 1 calc R . .
C3 C 0.8517(2) 0.7884(2) 0.7889(2) 0.0528(9) Uani 1 1 d . . .
H3 H 0.8006 0.7772 0.7892 0.063 Uiso 1 1 calc R . .
C4 C 0.8790(2) 0.8483(2) 0.8236(2) 0.0458(8) Uani 1 1 d . . .
C5 C 0.9565(2) 0.86037(19) 0.82282(18) 0.0429(7) Uani 1 1 d . . .
C6 C 0.9903(2) 0.9182(2) 0.85838(18) 0.0452(8) Uani 1 1 d . . .
C7 C 0.9464(2) 0.9677(2) 0.89497(17) 0.0433(7) Uani 1 1 d . . .
C8 C 0.9839(2) 1.0226(3) 0.9283(2) 0.0555(10) Uani 1 1 d . . .
H8 H 0.9571 1.0565 0.9524 0.067 Uiso 1 1 calc R . .
C9 C 1.0609(3) 1.0256(3) 0.9247(2) 0.0616(11) Uani 1 1 d . . .
H9 H 1.0866 1.0620 0.9465 0.074 Uiso 1 1 calc R . .
C10 C 1.1016(2) 0.9747(3) 0.8888(2) 0.0578(10) Uani 1 1 d . . .
H10 H 1.1540 0.9773 0.8882 0.069 Uiso 1 1 calc R . .
C11 C 0.8339(2) 0.8989(2) 0.8593(2) 0.0491(8) Uani 1 1 d . . .
C12 C 0.8676(2) 0.9563(2) 0.89230(18) 0.0464(8) Uani 1 1 d . . .
C13 C 0.7443(2) 0.9596(2) 0.9010(2) 0.0549(9) Uani 1 1 d . . .
C14 C 0.6697(3) 0.9860(3) 0.9266(3) 0.0737(14) Uani 1 1 d . . .
C15 C 0.6665(4) 1.0000(4) 0.9936(4) 0.098(2) Uani 1 1 d . . .
H15 H 0.7099 0.9948 1.0190 0.118 Uiso 1 1 calc R . .
C16 C 0.6010(5) 1.0211(7) 1.0232(6) 0.153(5) Uani 1 1 d . . .
H16 H 0.5991 1.0284 1.0686 0.184 Uiso 1 1 calc R . .
C17 C 0.5366(6) 1.0316(10) 0.9840(8) 0.194(7) Uani 1 1 d . . .
H17 H 0.4917 1.0464 1.0035 0.233 Uiso 1 1 calc R . .
C18 C 0.5396(4) 1.0203(4) 0.9180(6) 0.122(3) Uani 1 1 d . . .
H18 H 0.4968 1.0278 0.8922 0.146 Uiso 1 1 calc R . .
C19 C 0.6066(3) 0.9973(3) 0.8883(4) 0.0845(18) Uani 1 1 d . . .
C20 C 0.6021(3) 0.9876(3) 0.8167(5) 0.094(2) Uani 1 1 d . . .
C21 C 1.0798(2) 0.7396(2) 0.90356(19) 0.0477(8) Uani 1 1 d . . .
H21 H 1.0305 0.7379 0.8879 0.057 Uiso 1 1 calc R . .
C22 C 1.1007(2) 0.6939(2) 0.9550(2) 0.0485(8) Uani 1 1 d . . .
H22 H 1.0656 0.6621 0.9723 0.058 Uiso 1 1 calc R . .
C23 C 1.1728(2) 0.6955(2) 0.98034(18) 0.0469(8) Uani 1 1 d . . .
H23 H 1.1875 0.6648 1.0142 0.056 Uiso 1 1 calc R . .
C24 C 1.2239(2) 0.7458(2) 0.95256(18) 0.0434(7) Uani 1 1 d . . .
C25 C 1.19900(19) 0.7896(2) 0.90167(18) 0.0427(7) Uani 1 1 d . . .
C26 C 1.2476(2) 0.8408(2) 0.87014(18) 0.0448(8) Uani 1 1 d . . .
C27 C 1.3221(2) 0.8508(2) 0.89238(19) 0.0455(8) Uani 1 1 d . . .
C28 C 1.3653(2) 0.9027(2) 0.8590(2) 0.0514(9) Uani 1 1 d . . .
H28 H 1.4147 0.9123 0.8719 0.062 Uiso 1 1 calc R . .
C29 C 1.3331(2) 0.9391(2) 0.8067(2) 0.0556(9) Uani 1 1 d . . .
H29 H 1.3612 0.9731 0.7840 0.067 Uiso 1 1 calc R . .
C30 C 1.2601(2) 0.9256(2) 0.7877(2) 0.0518(9) Uani 1 1 d . . .
H30 H 1.2402 0.9509 0.7522 0.062 Uiso 1 1 calc R . .
C31 C 1.2998(2) 0.7543(2) 0.97228(19) 0.0472(8) Uani 1 1 d . . .
C32 C 1.34734(19) 0.8060(2) 0.94392(18) 0.0450(8) Uani 1 1 d . . .
C33 C 1.4112(2) 0.7483(2) 1.01543(18) 0.0481(8) Uani 1 1 d . . .
C34 C 1.4762(2) 0.7207(2) 1.0520(2) 0.0519(9) Uani 1 1 d . . .
C35 C 1.5066(3) 0.6563(3) 1.0328(2) 0.0569(10) Uani 1 1 d . . .
H35 H 1.4815 0.6291 1.0012 0.068 Uiso 1 1 calc R . .
C36 C 1.5737(3) 0.6307(3) 1.0593(3) 0.0729(13) Uani 1 1 d . . .
H36 H 1.5939 0.5875 1.0450 0.088 Uiso 1 1 calc R . .
C37 C 1.6098(3) 0.6701(4) 1.1068(3) 0.0768(15) Uani 1 1 d . . .
H37 H 1.6551 0.6537 1.1244 0.092 Uiso 1 1 calc R . .
C38 C 1.5798(3) 0.7336(3) 1.1288(3) 0.0698(13) Uani 1 1 d . . .
H38 H 1.6048 0.7597 1.1612 0.084 Uiso 1 1 calc R . .
C39 C 1.5116(2) 0.7593(3) 1.10251(19) 0.0551(10) Uani 1 1 d . . .
C40 C 1.4815(3) 0.8284(3) 1.1277(2) 0.0701(14) Uani 1 1 d . . .
C41 C 1.1678(2) 0.7066(2) 0.7494(2) 0.0465(8) Uani 1 1 d . . .
H41 H 1.1610 0.6885 0.7918 0.056 Uiso 1 1 calc R . .
C42 C 1.1965(3) 0.6618(2) 0.6996(2) 0.0567(10) Uani 1 1 d . . .
H42 H 1.2089 0.6147 0.7096 0.068 Uiso 1 1 calc R . .
C43 C 1.2064(3) 0.6863(3) 0.6377(2) 0.0653(12) Uani 1 1 d . . .
H43 H 1.2259 0.6564 0.6052 0.078 Uiso 1 1 calc R . .
C44 C 1.1872(3) 0.7565(3) 0.6229(2) 0.0578(10) Uani 1 1 d . . .
C45 C 1.1585(2) 0.7998(2) 0.67409(19) 0.0459(8) Uani 1 1 d . . .
C46 C 1.1342(2) 0.8721(2) 0.66290(19) 0.0453(8) Uani 1 1 d . . .
C47 C 1.1382(2) 0.9035(2) 0.6004(2) 0.0497(9) Uani 1 1 d . . .
C48 C 1.1119(2) 0.9741(2) 0.5948(2) 0.0550(9) Uani 1 1 d . . .
H48 H 1.1138 0.9978 0.5544 0.066 Uiso 1 1 calc R . .
C49 C 1.0836(3) 1.0078(2) 0.6493(2) 0.0568(10) Uani 1 1 d . . .
H49 H 1.0655 1.0544 0.6461 0.068 Uiso 1 1 calc R . .
C50 C 1.0821(2) 0.9720(2) 0.7097(2) 0.0502(9) Uani 1 1 d . . .
H50 H 1.0627 0.9961 0.7462 0.060 Uiso 1 1 calc R . .
C51 C 1.1923(3) 0.7913(3) 0.5595(2) 0.0649(12) Uani 1 1 d . . .
C52 C 1.1701(3) 0.8604(3) 0.5494(2) 0.0578(10) Uani 1 1 d . . .
C53 C 1.2077(4) 0.8137(4) 0.4578(3) 0.093(2) Uani 1 1 d . . .
C54 C 1.2257(6) 0.8040(5) 0.3871(3) 0.123(3) Uani 1 1 d . . .
C55 C 1.2735(9) 0.8341(5) 0.3562(6) 0.179(7) Uani 1 1 d . . .
H55 H 1.3009 0.8677 0.3801 0.215 Uiso 1 1 calc R . .
C56 C 1.2957(6) 0.8272(4) 0.2883(4) 0.115(3) Uani 1 1 d . . .
H56 H 1.3319 0.8572 0.2698 0.139 Uiso 1 1 calc R . .
C57 C 1.2627(7) 0.7766(7) 0.2530(5) 0.136(4) Uani 1 1 d . . .
H57 H 1.2726 0.7745 0.2079 0.164 Uiso 1 1 calc R . .
C58 C 1.2125(9) 0.7250(7) 0.2810(5) 0.155(4) Uani 1 1 d . . .
H58 H 1.1984 0.6840 0.2580 0.186 Uiso 1 1 calc R . .
C59 C 1.1850(6) 0.7394(5) 0.3460(4) 0.112(2) Uani 1 1 d . . .
C60 C 1.1286(9) 0.6918(8) 0.3704(5) 0.163(5) Uani 1 1 d . . .
N1 N 1.00632(17) 0.81864(16) 0.78939(15) 0.0438(6) Uani 1 1 d . . .
N2 N 1.06739(16) 0.92227(18) 0.85511(16) 0.0449(7) Uani 1 1 d . . .
N3 N 0.75675(19) 0.90226(19) 0.8643(2) 0.0556(8) Uani 1 1 d . . .
N4 N 0.80880(19) 0.9928(2) 0.92056(17) 0.0536(8) Uani 1 1 d . . .
N5 N 1.12717(17) 0.78492(18) 0.87649(15) 0.0444(7) Uani 1 1 d . . .
N6 N 1.21617(17) 0.87720(18) 0.81868(16) 0.0468(7) Uani 1 1 d . . .
N7 N 1.34179(17) 0.7158(2) 1.01822(16) 0.0508(8) Uani 1 1 d . . .
N8 N 1.41813(17) 0.8030(2) 0.97148(18) 0.0514(8) Uani 1 1 d . . .
N9 N 1.15004(16) 0.77463(18) 0.73704(16) 0.0442(7) Uani 1 1 d . . .
N10 N 1.10654(17) 0.90603(18) 0.71783(16) 0.0454(7) Uani 1 1 d . . .
N11 N 1.2166(3) 0.7609(3) 0.5004(2) 0.0930(18) Uani 1 1 d . . .
N12 N 1.1792(3) 0.8759(3) 0.4832(2) 0.0698(11) Uani 1 1 d . . .
F1 F 0.6670(2) 1.00051(19) 0.78475(19) 0.0886(9) Uani 1 1 d . . .
F2 F 0.5828(2) 0.9197(2) 0.7997(3) 0.1182(16) Uani 1 1 d . . .
F3 F 0.5514(3) 1.0289(3) 0.7864(3) 0.1333(19) Uani 1 1 d . . .
F4 F 1.5003(2) 0.88438(19) 1.09016(17) 0.0875(9) Uani 1 1 d . . .
F5 F 1.4053(2) 0.8291(2) 1.13149(18) 0.0891(10) Uani 1 1 d . . .
F6 F 1.5055(3) 0.8424(3) 1.18914(18) 0.1055(13) Uani 1 1 d . . .
F7 F 1.1566(5) 0.6324(3) 0.4065(3) 0.168(3) Uani 1 1 d . . .
F8 F 1.0786(4) 0.7235(5) 0.4091(3) 0.165(3) Uani 1 1 d . . .
F9 F 1.0861(6) 0.6607(5) 0.3209(4) 0.203(4) Uani 1 1 d . . .
C1S C 0.3073(6) 0.0645(6) 0.6678(8) 0.148(4) Uani 1 1 d . . .
H1S1 H 0.3257 0.0779 0.7107 0.222 Uiso 1 1 calc R . .
H1S2 H 0.3484 0.0641 0.6370 0.222 Uiso 1 1 calc R . .
H1S3 H 0.2852 0.0177 0.6701 0.222 Uiso 1 1 calc R . .
C2S C 0.2400(5) 0.1255(8) 0.6422(4) 0.173(6) Uani 1 1 d . . .
H2S1 H 0.1978 0.1265 0.6727 0.207 Uiso 1 1 calc R . .
H2S2 H 0.2614 0.1732 0.6394 0.207 Uiso 1 1 calc R . .
O1S O 0.2182(3) 0.1031(4) 0.5834(4) 0.138(3) Uani 1 1 d . . .
H1S H 0.1862 0.1305 0.5687 0.207 Uiso 1 1 calc R . .


_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 N1 1.956(3) . ?
Fe1 N2 1.961(3) . ?
Fe1 N6 1.971(3) . ?
Fe1 N10 1.973(3) . ?
Fe1 N9 1.976(3) . ?
Fe1 N5 1.979(3) . ?
C1 N1 1.359(5) . ?
C1 C2 1.368(6) . ?
C2 C3 1.373(7) . ?
C3 C4 1.407(6) . ?
C4 C5 1.392(5) . ?
C4 C11 1.433(6) . ?
C5 N1 1.359(5) . ?
C5 C6 1.431(5) . ?
C6 N2 1.370(5) . ?
C6 C7 1.417(5) . ?
C7 C8 1.396(6) . ?
C7 C12 1.415(5) . ?
C8 C9 1.367(6) . ?
C9 C10 1.398(7) . ?
C10 N2 1.337(5) . ?
C11 N3 1.372(5) . ?
C11 C12 1.397(6) . ?
C12 N4 1.370(5) . ?
C13 N3 1.322(6) . ?
C13 N4 1.360(6) . ?
C13 C14 1.502(6) . ?
C14 C19 1.376(9) . ?
C14 C15 1.384(10) . ?
C15 C16 1.364(10) . ?
C16 C17 1.402(19) . ?
C17 C18 1.356(18) . ?
C18 C19 1.399(9) . ?
C19 C20 1.463(11) . ?
C20 F3 1.333(7) . ?
C20 F1 1.341(8) . ?
C20 F2 1.358(7) . ?
C21 N5 1.312(5) . ?
C21 C22 1.397(6) . ?
C22 C23 1.378(5) . ?
C23 C24 1.421(5) . ?
C24 C25 1.388(5) . ?
C24 C31 1.412(5) . ?
C25 N5 1.374(5) . ?
C25 C26 1.437(5) . ?
C26 N6 1.363(5) . ?
C26 C27 1.407(5) . ?
C27 C28 1.409(6) . ?
C27 C32 1.411(5) . ?
C28 C29 1.382(6) . ?
C29 C30 1.373(5) . ?
C30 N6 1.348(5) . ?
C31 N7 1.392(5) . ?
C31 C32 1.404(5) . ?
C32 N8 1.374(5) . ?
C33 N8 1.361(6) . ?
C33 N7 1.372(5) . ?
C33 C34 1.464(5) . ?
C34 C35 1.373(7) . ?
C34 C39 1.400(6) . ?
C35 C36 1.391(6) . ?
C36 C37 1.369(8) . ?
C37 C38 1.374(8) . ?
C38 C39 1.404(6) . ?
C39 C40 1.487(7) . ?
C40 F4 1.335(7) . ?
C40 F6 1.341(6) . ?
C40 F5 1.353(6) . ?
C41 N9 1.333(5) . ?
C41 C42 1.406(6) . ?
C42 C43 1.346(7) . ?
C43 C44 1.387(7) . ?
C44 C45 1.411(6) . ?
C44 C51 1.441(6) . ?
C45 N9 1.367(5) . ?
C45 C46 1.435(6) . ?
C46 N10 1.371(5) . ?
C46 C47 1.397(5) . ?
C47 C48 1.405(6) . ?
C47 C52 1.426(6) . ?
C48 C49 1.366(7) . ?
C49 C50 1.393(6) . ?
C50 N10 1.318(5) . ?
C51 C52 1.366(7) . ?
C51 N11 1.393(6) . ?
C52 N12 1.381(5) . ?
C53 N11 1.320(8) . ?
C53 N12 1.366(8) . ?
C53 C54 1.477(8) . ?
C54 C55 1.193(12) . ?
C54 C59 1.635(14) . ?
C55 C56 1.437(11) . ?
C56 C57 1.321(14) . ?
C57 C58 1.430(17) . ?
C58 C59 1.429(14) . ?
C59 C60 1.427(14) . ?
C60 F8 1.323(15) . ?
C60 F9 1.382(13) . ?
C60 F7 1.418(17) . ?
C1S C2S 1.730(16) . ?
C2S O1S 1.319(13) . ?

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 Fe1 N2 82.66(12) . . ?
N1 Fe1 N6 174.04(13) . . ?
N2 Fe1 N6 93.53(13) . . ?
N1 Fe1 N10 91.49(13) . . ?
N2 Fe1 N10 94.15(14) . . ?
N6 Fe1 N10 93.37(13) . . ?
N1 Fe1 N9 94.13(13) . . ?
N2 Fe1 N9 175.30(13) . . ?
N6 Fe1 N9 89.94(13) . . ?
N10 Fe1 N9 82.46(14) . . ?
N1 Fe1 N5 92.60(13) . . ?
N2 Fe1 N5 90.99(13) . . ?
N6 Fe1 N5 82.86(13) . . ?
N10 Fe1 N5 173.80(13) . . ?
N9 Fe1 N5 92.59(13) . . ?
N1 C1 C2 122.2(4) . . ?
C1 C2 C3 120.9(4) . . ?
C2 C3 C4 118.6(4) . . ?
C5 C4 C3 117.5(3) . . ?
C5 C4 C11 116.6(3) . . ?
C3 C4 C11 125.8(3) . . ?
N1 C5 C4 123.7(3) . . ?
N1 C5 C6 114.3(3) . . ?
C4 C5 C6 122.0(3) . . ?
N2 C6 C7 122.4(3) . . ?
N2 C6 C5 115.8(3) . . ?
C7 C6 C5 121.8(3) . . ?
C8 C7 C12 126.9(4) . . ?
C8 C7 C6 118.1(3) . . ?
C12 C7 C6 115.1(3) . . ?
C9 C8 C7 118.7(4) . . ?
C8 C9 C10 120.9(4) . . ?
N2 C10 C9 122.0(4) . . ?
N3 C11 C12 110.8(4) . . ?
N3 C11 C4 128.5(4) . . ?
C12 C11 C4 120.7(3) . . ?
N4 C12 C11 104.9(3) . . ?
N4 C12 C7 131.3(4) . . ?
C11 C12 C7 123.8(3) . . ?
N3 C13 N4 113.1(4) . . ?
N3 C13 C14 127.3(4) . . ?
N4 C13 C14 119.4(4) . . ?
C19 C14 C15 119.3(5) . . ?
C19 C14 C13 124.9(6) . . ?
C15 C14 C13 115.8(6) . . ?
C16 C15 C14 121.3(9) . . ?
C15 C16 C17 119.0(11) . . ?
C18 C17 C16 120.3(8) . . ?
C17 C18 C19 120.3(10) . . ?
C14 C19 C18 119.7(8) . . ?
C14 C19 C20 125.7(5) . . ?
C18 C19 C20 114.6(7) . . ?
F3 C20 F1 104.6(7) . . ?
F3 C20 F2 104.7(5) . . ?
F1 C20 F2 105.2(5) . . ?
F3 C20 C19 114.9(6) . . ?
F1 C20 C19 114.1(5) . . ?
F2 C20 C19 112.4(7) . . ?
N5 C21 C22 122.4(4) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C23 C24 117.2(3) . . ?
C25 C24 C31 116.5(3) . . ?
C25 C24 C23 118.8(3) . . ?
C31 C24 C23 124.7(3) . . ?
N5 C25 C24 122.1(3) . . ?
N5 C25 C26 115.7(3) . . ?
C24 C25 C26 122.1(3) . . ?
N6 C26 C27 124.2(3) . . ?
N6 C26 C25 115.2(3) . . ?
C27 C26 C25 120.6(3) . . ?
C26 C27 C28 116.6(3) . . ?
C26 C27 C32 117.1(3) . . ?
C28 C27 C32 126.2(3) . . ?
C29 C28 C27 118.8(3) . . ?
C30 C29 C28 121.0(4) . . ?
N6 C30 C29 122.4(4) . . ?
N7 C31 C32 107.9(3) . . ?
N7 C31 C24 129.8(4) . . ?
C32 C31 C24 122.3(3) . . ?
N8 C32 C31 110.7(3) . . ?
N8 C32 C27 127.9(3) . . ?
C31 C32 C27 121.3(3) . . ?
N8 C33 N7 116.1(3) . . ?
N8 C33 C34 121.6(4) . . ?
N7 C33 C34 122.0(4) . . ?
C35 C34 C39 118.9(4) . . ?
C35 C34 C33 118.2(4) . . ?
C39 C34 C33 122.8(4) . . ?
C34 C35 C36 121.8(4) . . ?
C37 C36 C35 119.0(5) . . ?
C36 C37 C38 120.8(4) . . ?
C37 C38 C39 120.3(5) . . ?
C34 C39 C38 119.1(4) . . ?
C34 C39 C40 122.5(4) . . ?
C38 C39 C40 118.4(4) . . ?
F4 C40 F6 107.2(5) . . ?
F4 C40 F5 105.9(5) . . ?
F6 C40 F5 105.2(4) . . ?
F4 C40 C39 113.3(4) . . ?
F6 C40 C39 112.0(5) . . ?
F5 C40 C39 112.7(5) . . ?
N9 C41 C42 121.2(4) . . ?
C43 C42 C41 120.8(4) . . ?
C42 C43 C44 119.4(4) . . ?
C43 C44 C45 118.1(4) . . ?
C43 C44 C51 127.2(4) . . ?
C45 C44 C51 114.6(4) . . ?
N9 C45 C44 121.8(4) . . ?
N9 C45 C46 116.0(3) . . ?
C44 C45 C46 122.2(4) . . ?
N10 C46 C47 123.9(4) . . ?
N10 C46 C45 114.5(3) . . ?
C47 C46 C45 121.5(4) . . ?
C46 C47 C48 116.8(4) . . ?
C46 C47 C52 116.1(4) . . ?
C48 C47 C52 127.1(4) . . ?
C49 C48 C47 119.3(4) . . ?
C48 C49 C50 119.7(4) . . ?
N10 C50 C49 123.6(4) . . ?
C52 C51 N11 110.2(4) . . ?
C52 C51 C44 122.9(4) . . ?
N11 C51 C44 126.9(5) . . ?
C51 C52 N12 108.0(4) . . ?
C51 C52 C47 122.5(4) . . ?
N12 C52 C47 129.3(4) . . ?
N11 C53 N12 115.7(5) . . ?
N11 C53 C54 121.0(6) . . ?
N12 C53 C54 123.2(5) . . ?
C55 C54 C53 127.2(11) . . ?
C55 C54 C59 113.1(8) . . ?
C53 C54 C59 119.3(8) . . ?
C54 C55 C56 130.9(12) . . ?
C57 C56 C55 117.4(9) . . ?
C56 C57 C58 122.9(9) . . ?
C59 C58 C57 116.7(11) . . ?
C60 C59 C58 116.1(10) . . ?
C60 C59 C54 126.4(7) . . ?
C58 C59 C54 117.3(9) . . ?
F8 C60 F9 104.6(13) . . ?
F8 C60 F7 106.3(9) . . ?
F9 C60 F7 103.6(10) . . ?
F8 C60 C59 113.2(11) . . ?
F9 C60 C59 113.1(9) . . ?
F7 C60 C59 115.0(13) . . ?
C5 N1 C1 117.1(3) . . ?
C5 N1 Fe1 114.3(2) . . ?
C1 N1 Fe1 128.6(3) . . ?
C10 N2 C6 117.9(3) . . ?
C10 N2 Fe1 129.3(3) . . ?
C6 N2 Fe1 112.9(2) . . ?
C13 N3 C11 104.2(4) . . ?
C13 N4 C12 106.9(4) . . ?
C21 N5 C25 118.6(3) . . ?
C21 N5 Fe1 128.7(3) . . ?
C25 N5 Fe1 112.6(2) . . ?
C30 N6 C26 117.0(3) . . ?
C30 N6 Fe1 129.4(3) . . ?
C26 N6 Fe1 113.5(3) . . ?
C33 N7 C31 102.9(3) . . ?
C33 N8 C32 102.3(3) . . ?
C41 N9 C45 118.6(3) . . ?
C41 N9 Fe1 128.4(3) . . ?
C45 N9 Fe1 113.0(3) . . ?
C50 N10 C46 116.7(3) . . ?
C50 N10 Fe1 129.5(3) . . ?
C46 N10 Fe1 113.8(3) . . ?
C53 N11 C51 102.7(5) . . ?
C53 N12 C52 103.4(4) . . ?
O1S C2S C1S 105.3(12) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        73.41
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.069

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.080 0.000 0.793 2023 593 ' '
_platon_squeeze_details          
;
The unit cell contains disordered ethanol and water molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 2055 A3 containing about 593 electrons which corresponds to approximately 3 ethanol molecules and 7 water molecules per formula unit. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
# start Validation Reply Form
_vrf_CHEMW03_3                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert origins from the number of solvent molecules 
(3 ethanol, 7 water) calculated by using 
SQUEEZE/PLATON procedure and inserted in the 
empirical formula and molecular weight.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1835923'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H9 O4, C57 H33 N12 Fe, H2 O'
_chemical_formula_sum            'C57 H44 Fe N12 O5'
_chemical_formula_weight         1032.89

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R32

loop_
_symmetry_equiv_pos_as_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                   17.0059(2)
_cell_length_b                   17.0059(2)
_cell_length_c                   17.2491(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4320.12(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    5980
_cell_measurement_theta_min      5.1810
_cell_measurement_theta_max      73.1310

_exptl_crystal_description       cubic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    2.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82046
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.894
_oxdiff_exptl_absorpt_empirical_full_max 1.255
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6999
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         73.41
_reflns_number_total             1918
_reflns_number_gt                1915
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0716P)²+4.9192P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1918
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.1089
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.97303(15) 0.86242(16) 0.87982(13) 0.0247(5) Uani 1 1 d . . .
H1 H 1.0305 0.9033 0.8609 0.030 Uiso 1 1 calc R . .
C2 C 0.92351(17) 0.77709(17) 0.84449(13) 0.0286(5) Uani 1 1 d . . .
H2 H 0.9479 0.7624 0.8024 0.034 Uiso 1 1 calc R . .
C3 C 0.83858(15) 0.71485(15) 0.87210(13) 0.0262(5) Uani 1 1 d . . .
H3 H 0.8055 0.6579 0.8492 0.031 Uiso 1 1 calc R . .
C4 C 0.80289(16) 0.73894(15) 0.93536(13) 0.0229(4) Uani 1 1 d . . .
C5 C 0.85624(15) 0.82562(15) 0.96713(12) 0.0197(4) Uani 1 1 d . . .
C6 C 0.71555(16) 0.68360(15) 0.97018(13) 0.0256(5) Uani 1 1 d . . .
C7 C 0.5804(2) 0.5804(2) 1.0000 0.0301(7) Uani 1 2 d S . .
C8 C 0.4934(2) 0.4934(2) 1.0000 0.0380(8) Uani 1 2 d S . .
C9 C 0.4884(2) 0.4155(2) 0.96918(18) 0.0515(9) Uani 1 1 d . . .
H9 H 0.5399 0.4178 0.9483 0.062 Uiso 1 1 calc R . .
C10 C 0.9279(4) 0.5935(3) 0.9696(2) 0.0725(14) Uani 1 1 d . . .
H10 H 0.8788 0.5963 0.9490 0.087 Uiso 1 1 calc R . .
C11 C 1.0000 0.6706(3) 1.0000 0.083(2) Uani 1 2 d S . .
H11 H 1.0000 0.7253 1.0000 0.100 Uiso 1 2 calc SR . .
N1 N 0.94034(14) 0.88688(11) 0.93979(9) 0.0200(3) Uani 1 1 d . . .
N2 N 0.64967(14) 0.59663(14) 0.95202(12) 0.0280(5) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.8333 0.231(10) Uani 1 6 d S . .
O2 O 0.6667 0.49229(18) 0.8333 0.0441(7) Uani 1 2 d S . .
Fe1 Fe 1.0000 1.0000 1.0000 0.0175(2) Uani 1 6 d S . .
H2S H 0.661(4) 0.530(3) 0.869(2) 0.088(15) Uiso 1 1 d . . .


_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
C1 N1 1.336(3) . ?
C1 C2 1.401(3) . ?
C2 C3 1.380(3) . ?
C3 C4 1.406(3) . ?
C4 C5 1.400(3) . ?
C4 C6 1.433(3) . ?
C5 N1 1.365(3) . ?
C5 C5 1.449(4) 6_557 ?
C6 N2 1.372(3) . ?
C6 C6 1.394(5) 6_557 ?
C7 N2 1.350(3) 6_557 ?
C7 N2 1.350(3) . ?
C7 C8 1.479(5) . ?
C8 C9 1.390(4) . ?
C8 C9 1.390(4) 6_557 ?
C9 C10 1.385(4) 2_655 ?
C10 C11 1.375(5) . ?
C10 C9 1.385(4) 3_665 ?
C11 C10 1.375(5) 5_767 ?
N1 Fe1 1.9639(16) . ?
Fe1 N1 1.9638(16) 2_765 ?
Fe1 N1 1.9639(16) 4_677 ?
Fe1 N1 1.9639(16) 3_675 ?
Fe1 N1 1.9639(16) 6_557 ?
Fe1 N1 1.9640(16) 5_767 ?

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 C1 C2 122.1(2) . . ?
C3 C2 C1 120.0(2) . . ?
C2 C3 C4 118.9(2) . . ?
C5 C4 C3 117.6(2) . . ?
C5 C4 C6 116.1(2) . . ?
C3 C4 C6 126.2(2) . . ?
N1 C5 C4 123.27(19) . . ?
N1 C5 C5 115.07(11) . 6_557 ?
C4 C5 C5 121.65(13) . 6_557 ?
N2 C6 C6 108.73(14) . 6_557 ?
N2 C6 C4 129.2(2) . . ?
C6 C6 C4 122.08(13) 6_557 . ?
N2 C7 N2 114.9(3) 6_557 . ?
N2 C7 C8 122.56(16) 6_557 . ?
N2 C7 C8 122.56(16) . . ?
C9 C8 C9 119.0(4) . 6_557 ?
C9 C8 C7 120.5(2) . . ?
C9 C8 C7 120.5(2) 6_557 . ?
C10 C9 C8 119.9(4) 2_655 . ?
C11 C10 C9 121.1(4) . 3_665 ?
C10 C11 C10 118.9(5) 5_767 . ?
C1 N1 C5 118.06(17) . . ?
C1 N1 Fe1 128.54(16) . . ?
C5 N1 Fe1 113.32(14) . . ?
C7 N2 C6 103.8(2) . . ?
N1 Fe1 N1 87.69(12) 2_765 4_677 ?
N1 Fe1 N1 94.62(6) 2_765 . ?
N1 Fe1 N1 176.92(13) 4_677 . ?
N1 Fe1 N1 94.62(6) 2_765 3_675 ?
N1 Fe1 N1 83.15(12) 4_677 3_675 ?
N1 Fe1 N1 94.62(6) . 3_675 ?
N1 Fe1 N1 176.92(13) 2_765 6_557 ?
N1 Fe1 N1 94.62(6) 4_677 6_557 ?
N1 Fe1 N1 83.15(12) . 6_557 ?
N1 Fe1 N1 87.69(12) 3_675 6_557 ?
N1 Fe1 N1 83.15(12) 2_765 5_767 ?
N1 Fe1 N1 94.62(6) 4_677 5_767 ?
N1 Fe1 N1 87.69(12) . 5_767 ?
N1 Fe1 N1 176.92(14) 3_675 5_767 ?
N1 Fe1 N1 94.62(6) 6_557 5_767 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        73.41
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.056

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.009 -0.009 0.167 390 11 ' '
2 -0.006 -0.004 0.833 390 11 ' '
3 -0.024 0.483 0.500 390 11 ' '
_platon_squeeze_details          
;
The unit cell contains disordered solvent molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 1171 A3 containing about 32 electrons which corresponds to approximately 1 water molecule per formula unit. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1835927'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H31 N12 F9 Co, C4 H12 O2, H4 O2'
_chemical_formula_sum            'C64 H47 Co F9 N12 O4'
_chemical_formula_weight         1278.07

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   18.1082(8)
_cell_length_b                   15.7956(5)
_cell_length_c                   20.1176(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.471(4)
_cell_angle_gamma                90.00
_cell_volume                     5658.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    4395
_cell_measurement_theta_min      2.9880
_cell_measurement_theta_max      70.6850

_exptl_crystal_description       prismatic
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2620
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.825
_oxdiff_exptl_absorpt_empirical_full_max 1.151
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23812
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         73.58
_reflns_number_total             11125
_reflns_number_gt                6683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1497P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11125
_refine_ls_number_parameters     723
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2542
_refine_ls_wR_factor_gt          0.2246
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1307(3) 0.1256(3) 0.3898(2) 0.0772(15) Uani 1 1 d . . .
H1 H 0.1343 0.1565 0.3512 0.093 Uiso 1 1 calc R . .
C2 C 0.0946(4) 0.0473(4) 0.3833(3) 0.094(2) Uani 1 1 d . . .
H2 H 0.0746 0.0267 0.3406 0.113 Uiso 1 1 calc R . .
C3 C 0.0886(4) 0.0008(4) 0.4390(2) 0.0887(18) Uani 1 1 d . . .
H3 H 0.0654 -0.0520 0.4343 0.106 Uiso 1 1 calc R . .
C4 C 0.1175(3) 0.0328(3) 0.5035(2) 0.0701(13) Uani 1 1 d . . .
C5 C 0.1524(3) 0.1115(3) 0.5062(2) 0.0648(12) Uani 1 1 d . . .
C6 C 0.1821(3) 0.1518(3) 0.5701(2) 0.0619(11) Uani 1 1 d . . .
C7 C 0.1776(3) 0.1150(3) 0.6312(2) 0.0644(12) Uani 1 1 d . . .
C8 C 0.2054(3) 0.1624(3) 0.6909(2) 0.0723(13) Uani 1 1 d . . .
H8 H 0.2029 0.1406 0.7334 0.087 Uiso 1 1 calc R . .
C9 C 0.2354(3) 0.2400(3) 0.6842(2) 0.0752(15) Uani 1 1 d . . .
H9 H 0.2526 0.2722 0.7227 0.090 Uiso 1 1 calc R . .
C10 C 0.2409(3) 0.2725(3) 0.6208(2) 0.0675(12) Uani 1 1 d . . .
H10 H 0.2635 0.3249 0.6176 0.081 Uiso 1 1 calc R . .
C11 C 0.1161(3) -0.0072(3) 0.5677(2) 0.0677(12) Uani 1 1 d . . .
C12 C 0.1447(3) 0.0323(3) 0.6292(2) 0.0661(12) Uani 1 1 d . . .
C13 C 0.1049(3) -0.0894(3) 0.6473(2) 0.0687(12) Uani 1 1 d . . .
C14 C 0.0871(3) -0.1639(3) 0.6878(2) 0.0650(12) Uani 1 1 d . . .
C15 C 0.0456(3) -0.1477(3) 0.7384(3) 0.0765(14) Uani 1 1 d . . .
H15 H 0.0302 -0.0928 0.7454 0.092 Uiso 1 1 calc R . .
C16 C 0.0274(3) -0.2127(3) 0.7781(2) 0.0746(13) Uani 1 1 d . . .
H16 H -0.0012 -0.2013 0.8111 0.090 Uiso 1 1 calc R . .
C17 C 0.0503(3) -0.2929(3) 0.7699(3) 0.0709(13) Uani 1 1 d . . .
H17 H 0.0374 -0.3361 0.7971 0.085 Uiso 1 1 calc R . .
C18 C 0.0931(3) -0.3111(3) 0.7209(3) 0.0713(13) Uani 1 1 d . . .
H18 H 0.1097 -0.3661 0.7158 0.086 Uiso 1 1 calc R . .
C19 C 0.1111(3) -0.2464(3) 0.6793(2) 0.0654(12) Uani 1 1 d . . .
C20 C 0.1602(4) -0.2684(4) 0.6302(3) 0.0831(16) Uani 1 1 d . . .
C21 C 0.2678(3) 0.4363(3) 0.5007(3) 0.0736(13) Uani 1 1 d . . .
H21 H 0.2177 0.4527 0.4894 0.088 Uiso 1 1 calc R . .
C22 C 0.3216(3) 0.4969(3) 0.5195(3) 0.0843(16) Uani 1 1 d . . .
H22 H 0.3073 0.5534 0.5195 0.101 Uiso 1 1 calc R . .
C23 C 0.3957(3) 0.4763(3) 0.5384(3) 0.0764(14) Uani 1 1 d . . .
H23 H 0.4317 0.5180 0.5517 0.092 Uiso 1 1 calc R . .
C24 C 0.4164(3) 0.3903(3) 0.5374(2) 0.0630(11) Uani 1 1 d . . .
C25 C 0.3588(3) 0.3313(3) 0.5152(2) 0.0594(10) Uani 1 1 d . . .
C26 C 0.3734(3) 0.2433(2) 0.5098(2) 0.0579(11) Uani 1 1 d . . .
C27 C 0.4461(3) 0.2106(3) 0.5270(2) 0.0612(11) Uani 1 1 d . . .
C28 C 0.4544(3) 0.1226(3) 0.5195(3) 0.0750(14) Uani 1 1 d . . .
H28 H 0.5012 0.0973 0.5323 0.090 Uiso 1 1 calc R . .
C29 C 0.3935(3) 0.0749(3) 0.4934(3) 0.0809(16) Uani 1 1 d . . .
H29 H 0.3990 0.0171 0.4869 0.097 Uiso 1 1 calc R . .
C30 C 0.3232(3) 0.1123(3) 0.4765(3) 0.0724(14) Uani 1 1 d . . .
H30 H 0.2821 0.0786 0.4589 0.087 Uiso 1 1 calc R . .
C31 C 0.4902(3) 0.3564(3) 0.5566(2) 0.0618(11) Uani 1 1 d . . .
C32 C 0.5044(3) 0.2696(3) 0.5518(2) 0.0591(10) Uani 1 1 d . . .
C33 C 0.6065(3) 0.3322(3) 0.5896(2) 0.0615(11) Uani 1 1 d . . .
C34 C 0.6891(3) 0.3425(3) 0.6091(2) 0.0663(12) Uani 1 1 d . . .
C35 C 0.7326(3) 0.2957(4) 0.5724(3) 0.0872(16) Uani 1 1 d . . .
H35 H 0.7088 0.2596 0.5387 0.105 Uiso 1 1 calc R . .
C36 C 0.8103(3) 0.3009(5) 0.5842(4) 0.102(2) Uani 1 1 d . . .
H36 H 0.8377 0.2690 0.5583 0.122 Uiso 1 1 calc R . .
C37 C 0.8466(4) 0.3530(5) 0.6339(4) 0.0965(19) Uani 1 1 d . . .
H37 H 0.8986 0.3580 0.6412 0.116 Uiso 1 1 calc R . .
C38 C 0.8058(3) 0.3977(4) 0.6728(3) 0.0863(17) Uani 1 1 d . . .
H38 H 0.8305 0.4318 0.7075 0.104 Uiso 1 1 calc R . .
C39 C 0.7270(3) 0.3929(3) 0.6612(3) 0.0734(13) Uani 1 1 d . . .
C40 C 0.6875(4) 0.4422(5) 0.7064(4) 0.111(2) Uani 1 1 d . . .
C41 C 0.2699(3) 0.2601(3) 0.3398(3) 0.0694(13) Uani 1 1 d . . .
H41 H 0.3080 0.2225 0.3573 0.083 Uiso 1 1 calc R . .
C42 C 0.2648(3) 0.2894(3) 0.2739(3) 0.0727(13) Uani 1 1 d . . .
H42 H 0.3003 0.2724 0.2485 0.087 Uiso 1 1 calc R . .
C43 C 0.2083(3) 0.3428(3) 0.2461(2) 0.0642(11) Uani 1 1 d . . .
H43 H 0.2047 0.3615 0.2018 0.077 Uiso 1 1 calc R . .
C44 C 0.1561(3) 0.3691(3) 0.2848(2) 0.0592(11) Uani 1 1 d . . .
C45 C 0.1642(2) 0.3377(3) 0.3516(2) 0.0582(10) Uani 1 1 d . . .
C46 C 0.1147(3) 0.3598(3) 0.3954(2) 0.0609(11) Uani 1 1 d . . .
C47 C 0.0527(2) 0.4140(3) 0.3761(2) 0.0595(11) Uani 1 1 d . . .
C48 C 0.0059(3) 0.4287(3) 0.4223(2) 0.0669(12) Uani 1 1 d . . .
H48 H -0.0360 0.4633 0.4107 0.080 Uiso 1 1 calc R . .
C49 C 0.0218(3) 0.3920(3) 0.4855(3) 0.0684(12) Uani 1 1 d . . .
H49 H -0.0097 0.4010 0.5165 0.082 Uiso 1 1 calc R . .
C50 C 0.0853(3) 0.3412(3) 0.5025(2) 0.0662(12) Uani 1 1 d . . .
H50 H 0.0965 0.3182 0.5457 0.079 Uiso 1 1 calc R . .
C51 C 0.0943(3) 0.4268(2) 0.2655(2) 0.0584(11) Uani 1 1 d . . .
C52 C 0.0459(2) 0.4484(3) 0.3095(2) 0.0577(10) Uani 1 1 d . . .
C53 C 0.0165(3) 0.5162(3) 0.2170(2) 0.0728(14) Uani 1 1 d . . .
C54 C -0.0085(2) 0.5943(3) 0.1719(2) 0.0365(13) Uiso 0.50 1 d PG A 1
C55 C 0.0407(2) 0.6611(4) 0.1684(3) 0.056(3) Uiso 0.50 1 d PG A 1
H55 H 0.0909 0.6562 0.1886 0.067 Uiso 0.50 1 calc PR A 1
C56 C 0.0147(3) 0.7351(3) 0.1346(4) 0.063(2) Uiso 0.50 1 d PG A 1
H56 H 0.0476 0.7797 0.1322 0.076 Uiso 0.50 1 calc PR A 1
C57 C -0.0604(3) 0.7423(3) 0.1044(3) 0.0565(19) Uiso 0.50 1 d PG A 1
H57 H -0.0778 0.7918 0.0818 0.068 Uiso 0.50 1 calc PR A 1
C58 C -0.1096(2) 0.6756(3) 0.1079(3) 0.0489(17) Uiso 0.50 1 d PG A 1
H58 H -0.1598 0.6804 0.0877 0.059 Uiso 0.50 1 calc PR A 1
C59 C -0.0836(2) 0.6016(3) 0.1417(2) 0.0445(15) Uiso 0.50 1 d PG A 1
C60 C -0.1374(4) 0.5314(5) 0.1477(4) 0.048(2) Uiso 0.50 1 d P A 1
F7 F -0.1709(4) 0.5443(4) 0.2023(3) 0.0873(17) Uiso 0.50 1 d P A 1
F8 F -0.1150(3) 0.4559(4) 0.1468(3) 0.0771(15) Uiso 0.50 1 d P A 1
F9 F -0.1967(4) 0.5366(5) 0.0907(4) 0.0819(17) Uiso 0.50 1 d P A 1
C54B C -0.0587(5) 0.5527(5) 0.1699(4) 0.079(3) Uiso 0.50 1 d PG A 2
C55B C -0.1322(5) 0.5228(6) 0.1568(5) 0.201(15) Uiso 0.50 1 d PG A 2
H55B H -0.1458 0.4771 0.1810 0.241 Uiso 0.50 1 calc PR A 2
C56B C -0.1852(4) 0.5614(7) 0.1074(5) 0.101(5) Uiso 0.50 1 d PG A 2
H56B H -0.2343 0.5414 0.0987 0.121 Uiso 0.50 1 calc PR A 2
C57B C -0.1648(4) 0.6297(6) 0.0712(4) 0.091(3) Uiso 0.50 1 d PG A 2
H57B H -0.2003 0.6555 0.0382 0.109 Uiso 0.50 1 calc PR A 2
C58B C -0.0914(4) 0.6596(4) 0.0843(4) 0.075(3) Uiso 0.50 1 d PG A 2
H58B H -0.0778 0.7053 0.0600 0.090 Uiso 0.50 1 calc PR A 2
C59B C -0.0383(3) 0.6211(5) 0.1336(4) 0.079(3) Uiso 0.50 1 d PG A 2
C60B C 0.0364(7) 0.6571(8) 0.1525(8) 0.072(4) Uiso 0.50 1 d P A 2
F7B F 0.0961(5) 0.6183(6) 0.1430(5) 0.123(3) Uiso 0.50 1 d P A 2
F8B F 0.0521(5) 0.6807(6) 0.2211(5) 0.122(3) Uiso 0.50 1 d P A 2
F9B F 0.0390(5) 0.7378(5) 0.1221(5) 0.109(2) Uiso 0.50 1 d P A 2
N1 N 0.1601(2) 0.1570(2) 0.45034(18) 0.0625(9) Uani 1 1 d . . .
N2 N 0.2145(2) 0.2296(2) 0.56509(18) 0.0618(9) Uani 1 1 d . . .
N3 N 0.0913(3) -0.0865(2) 0.57943(19) 0.0714(11) Uani 1 1 d . . .
N4 N 0.1361(3) -0.0204(2) 0.67970(18) 0.0679(10) Uani 1 1 d . . .
N5 N 0.2852(2) 0.3543(2) 0.4981(2) 0.0658(10) Uani 1 1 d . . .
N6 N 0.3126(2) 0.1946(2) 0.48463(19) 0.0634(10) Uani 1 1 d . . .
N7 N 0.5568(2) 0.3968(2) 0.5808(2) 0.0646(9) Uani 1 1 d . . .
N8 N 0.5784(2) 0.2548(2) 0.57275(19) 0.0594(9) Uani 1 1 d . . .
N9 N 0.2213(2) 0.2848(2) 0.3781(2) 0.0622(9) Uani 1 1 d . . .
N10 N 0.1299(2) 0.3249(2) 0.45941(19) 0.0612(9) Uani 1 1 d . . .
N11 N 0.0742(2) 0.4704(2) 0.20606(18) 0.0655(10) Uani 1 1 d . A .
N12 N -0.0048(2) 0.5054(2) 0.27787(19) 0.0669(10) Uani 1 1 d . A .
H12 H -0.0414 0.5290 0.2928 0.080 Uiso 1 1 calc R . .
F1 F 0.2156(2) -0.2124(3) 0.6312(2) 0.1039(11) Uani 1 1 d . . .
F2 F 0.1243(2) -0.2736(2) 0.56666(16) 0.0983(10) Uani 1 1 d . . .
F3 F 0.1940(3) -0.3436(2) 0.6436(2) 0.1137(13) Uani 1 1 d . . .
F4 F 0.6287(2) 0.4022(3) 0.72293(18) 0.1138(13) Uani 1 1 d . . .
F5 F 0.6620(3) 0.5174(3) 0.6781(3) 0.157(2) Uani 1 1 d . . .
F6 F 0.7326(3) 0.4601(4) 0.7647(3) 0.175(3) Uani 1 1 d . . .
Co1 Co 0.22008(4) 0.25757(4) 0.47187(4) 0.0603(2) Uani 1 1 d . . .
O1S O 0.3636(2) 0.9112(2) 0.40630(16) 0.0743(9) Uani 1 1 d . . .
O2S O 0.0052(3) 0.8182(3) 0.4746(3) 0.1272(18) Uani 1 1 d . . .


_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
C1 N1 1.333(6) . ?
C1 C2 1.393(7) . ?
C2 C3 1.361(7) . ?
C3 C4 1.401(6) . ?
C4 C5 1.392(6) . ?
C4 C11 1.441(6) . ?
C5 N1 1.362(6) . ?
C5 C6 1.448(6) . ?
C6 N2 1.372(5) . ?
C6 C7 1.377(6) . ?
C7 C8 1.427(6) . ?
C7 C12 1.434(6) . ?
C8 C9 1.358(7) . ?
C9 C10 1.396(8) . ?
C10 N2 1.323(6) . ?
C11 N3 1.366(6) . ?
C11 C12 1.398(6) . ?
C12 N4 1.344(6) . ?
C13 N4 1.341(6) . ?
C13 N3 1.344(6) . ?
C13 C14 1.498(6) . ?
C14 C19 1.395(7) . ?
C14 C15 1.395(8) . ?
C15 C16 1.377(7) . ?
C16 C17 1.353(8) . ?
C17 C18 1.391(8) . ?
C18 C19 1.396(7) . ?
C19 C20 1.484(9) . ?
C20 F2 1.328(7) . ?
C20 F1 1.335(7) . ?
C20 F3 1.342(6) . ?
C21 N5 1.337(6) . ?
C21 C22 1.369(7) . ?
C22 C23 1.367(8) . ?
C23 C24 1.411(6) . ?
C24 C25 1.410(6) . ?
C24 C31 1.425(7) . ?
C25 N5 1.363(6) . ?
C25 C26 1.423(6) . ?
C26 N6 1.363(5) . ?
C26 C27 1.399(6) . ?
C27 C28 1.409(6) . ?
C27 C32 1.428(6) . ?
C28 C29 1.359(7) . ?
C29 C30 1.389(7) . ?
C30 N6 1.329(6) . ?
C31 N7 1.374(6) . ?
C31 C32 1.401(6) . ?
C32 N8 1.350(6) . ?
C33 N8 1.343(5) . ?
C33 N7 1.349(6) . ?
C33 C34 1.485(7) . ?
C34 C35 1.387(8) . ?
C34 C39 1.393(6) . ?
C35 C36 1.385(8) . ?
C36 C37 1.368(9) . ?
C37 C38 1.366(9) . ?
C38 C39 1.405(8) . ?
C39 C40 1.477(9) . ?
C40 F6 1.331(8) . ?
C40 F4 1.331(8) . ?
C40 F5 1.361(10) . ?
C41 N9 1.331(7) . ?
C41 C42 1.391(7) . ?
C42 C43 1.366(6) . ?
C43 C44 1.393(7) . ?
C44 C45 1.414(6) . ?
C44 C51 1.442(6) . ?
C45 N9 1.360(5) . ?
C45 C46 1.410(7) . ?
C46 N10 1.382(6) . ?
C46 C47 1.410(6) . ?
C47 C48 1.386(7) . ?
C47 C52 1.431(6) . ?
C48 C49 1.379(7) . ?
C49 C50 1.393(7) . ?
C50 N10 1.313(7) . ?
C51 N11 1.371(5) . ?
C51 C52 1.395(7) . ?
C52 N12 1.359(5) . ?
C53 N11 1.322(6) . ?
C53 N12 1.360(7) . ?
C53 C54 1.549(6) . ?
C53 C54B 1.617(8) . ?
C54 C55 1.3900 . ?
C54 C59 1.3900 . ?
C55 C56 1.3900 . ?
C56 C57 1.3900 . ?
C57 C58 1.3900 . ?
C58 C59 1.3900 . ?
C59 C60 1.494(9) . ?
C60 F8 1.262(10) . ?
C60 F7 1.364(10) . ?
C60 F9 1.424(11) . ?
C54B C55B 1.3900 . ?
C54B C59B 1.3900 . ?
C55B C56B 1.3900 . ?
C56B C57B 1.3900 . ?
C57B C58B 1.3900 . ?
C58B C59B 1.3900 . ?
C59B C60B 1.454(14) . ?
C60B F7B 1.287(14) . ?
C60B F8B 1.408(17) . ?
C60B F9B 1.418(14) . ?
N1 Co1 1.928(4) . ?
N2 Co1 1.947(4) . ?
N5 Co1 1.944(4) . ?
N6 Co1 1.925(4) . ?
N9 Co1 1.939(4) . ?
N10 Co1 1.927(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 C1 C2 121.3(4) . . ?
C3 C2 C1 120.6(5) . . ?
C2 C3 C4 119.6(5) . . ?
C5 C4 C3 116.7(4) . . ?
C5 C4 C11 115.9(4) . . ?
C3 C4 C11 127.3(4) . . ?
N1 C5 C4 123.6(4) . . ?
N1 C5 C6 115.0(4) . . ?
C4 C5 C6 121.4(4) . . ?
N2 C6 C7 122.6(4) . . ?
N2 C6 C5 115.1(4) . . ?
C7 C6 C5 122.3(4) . . ?
C6 C7 C8 117.4(4) . . ?
C6 C7 C12 116.8(4) . . ?
C8 C7 C12 125.7(4) . . ?
C9 C8 C7 118.5(5) . . ?
C8 C9 C10 121.3(4) . . ?
N2 C10 C9 120.7(4) . . ?
N3 C11 C12 109.6(4) . . ?
N3 C11 C4 128.1(4) . . ?
C12 C11 C4 122.3(4) . . ?
N4 C12 C11 108.6(4) . . ?
N4 C12 C7 130.2(4) . . ?
C11 C12 C7 121.1(4) . . ?
N4 C13 N3 116.6(4) . . ?
N4 C13 C14 119.2(4) . . ?
N3 C13 C14 124.2(4) . . ?
C19 C14 C15 118.8(4) . . ?
C19 C14 C13 124.4(5) . . ?
C15 C14 C13 116.8(4) . . ?
C16 C15 C14 120.3(5) . . ?
C17 C16 C15 121.1(6) . . ?
C16 C17 C18 120.2(5) . . ?
C17 C18 C19 119.7(5) . . ?
C14 C19 C18 119.9(5) . . ?
C14 C19 C20 122.5(4) . . ?
C18 C19 C20 117.4(5) . . ?
F2 C20 F1 106.9(5) . . ?
F2 C20 F3 105.3(5) . . ?
F1 C20 F3 105.6(5) . . ?
F2 C20 C19 114.1(5) . . ?
F1 C20 C19 112.0(5) . . ?
F3 C20 C19 112.4(5) . . ?
N5 C21 C22 121.8(5) . . ?
C23 C22 C21 121.7(4) . . ?
C22 C23 C24 118.4(4) . . ?
C25 C24 C23 117.2(4) . . ?
C25 C24 C31 116.2(4) . . ?
C23 C24 C31 126.6(4) . . ?
N5 C25 C24 122.5(4) . . ?
N5 C25 C26 115.3(4) . . ?
C24 C25 C26 122.2(4) . . ?
N6 C26 C27 122.9(4) . . ?
N6 C26 C25 115.6(4) . . ?
C27 C26 C25 121.5(4) . . ?
C26 C27 C28 116.9(4) . . ?
C26 C27 C32 116.6(4) . . ?
C28 C27 C32 126.5(4) . . ?
C29 C28 C27 119.6(4) . . ?
C28 C29 C30 120.2(4) . . ?
N6 C30 C29 122.1(4) . . ?
N7 C31 C32 108.6(4) . . ?
N7 C31 C24 129.8(4) . . ?
C32 C31 C24 121.6(4) . . ?
N8 C32 C31 109.3(4) . . ?
N8 C32 C27 128.7(4) . . ?
C31 C32 C27 122.0(4) . . ?
N8 C33 N7 116.2(4) . . ?
N8 C33 C34 118.9(4) . . ?
N7 C33 C34 124.5(4) . . ?
C35 C34 C39 117.0(5) . . ?
C35 C34 C33 116.4(4) . . ?
C39 C34 C33 126.7(5) . . ?
C36 C35 C34 122.4(6) . . ?
C37 C36 C35 119.9(6) . . ?
C38 C37 C36 119.4(6) . . ?
C37 C38 C39 121.0(5) . . ?
C34 C39 C38 120.2(5) . . ?
C34 C39 C40 122.5(5) . . ?
C38 C39 C40 117.3(5) . . ?
F6 C40 F4 105.7(6) . . ?
F6 C40 F5 106.9(6) . . ?
F4 C40 F5 107.0(7) . . ?
F6 C40 C39 111.5(7) . . ?
F4 C40 C39 113.6(6) . . ?
F5 C40 C39 111.6(7) . . ?
N9 C41 C42 121.2(4) . . ?
C43 C42 C41 120.7(5) . . ?
C42 C43 C44 119.3(4) . . ?
C43 C44 C45 117.6(4) . . ?
C43 C44 C51 127.6(4) . . ?
C45 C44 C51 114.8(4) . . ?
N9 C45 C46 115.5(4) . . ?
N9 C45 C44 121.9(5) . . ?
C46 C45 C44 122.6(4) . . ?
N10 C46 C45 116.3(4) . . ?
N10 C46 C47 120.8(5) . . ?
C45 C46 C47 122.9(4) . . ?
C48 C47 C46 118.1(4) . . ?
C48 C47 C52 127.3(4) . . ?
C46 C47 C52 114.6(4) . . ?
C49 C48 C47 119.8(4) . . ?
C48 C49 C50 119.5(5) . . ?
N10 C50 C49 122.0(4) . . ?
N11 C51 C52 109.5(4) . . ?
N11 C51 C44 128.5(5) . . ?
C52 C51 C44 122.0(4) . . ?
N12 C52 C51 108.3(4) . . ?
N12 C52 C47 128.7(5) . . ?
C51 C52 C47 123.0(4) . . ?
N11 C53 N12 116.3(4) . . ?
N11 C53 C54 119.6(5) . . ?
N12 C53 C54 121.8(4) . . ?
N11 C53 C54B 134.8(5) . . ?
N12 C53 C54B 103.1(5) . . ?
C54 C53 C54B 41.3(3) . . ?
C55 C54 C59 120.0 . . ?
C55 C54 C53 120.8(4) . . ?
C59 C54 C53 118.7(4) . . ?
C56 C55 C54 120.0 . . ?
C55 C56 C57 120.0 . . ?
C56 C57 C58 120.0 . . ?
C57 C58 C59 120.0 . . ?
C58 C59 C54 120.0 . . ?
C58 C59 C60 119.7(4) . . ?
C54 C59 C60 120.3(4) . . ?
F8 C60 F7 110.0(7) . . ?
F8 C60 F9 103.9(7) . . ?
F7 C60 F9 105.1(6) . . ?
F8 C60 C59 119.0(7) . . ?
F7 C60 C59 110.3(6) . . ?
F9 C60 C59 107.4(6) . . ?
C55B C54B C59B 120.0 . . ?
C55B C54B C53 131.7(5) . . ?
C59B C54B C53 108.0(5) . . ?
C56B C55B C54B 120.0 . . ?
C57B C56B C55B 120.0 . . ?
C58B C57B C56B 120.0 . . ?
C57B C58B C59B 120.0 . . ?
C58B C59B C54B 120.0 . . ?
C58B C59B C60B 120.3(7) . . ?
C54B C59B C60B 119.4(7) . . ?
F7B C60B F8B 104.4(11) . . ?
F7B C60B F9B 105.6(10) . . ?
F8B C60B F9B 99.7(10) . . ?
F7B C60B C59B 122.8(11) . . ?
F8B C60B C59B 111.8(10) . . ?
F9B C60B C59B 110.0(10) . . ?
C1 N1 C5 118.2(4) . . ?
C1 N1 Co1 128.9(3) . . ?
C5 N1 Co1 112.8(3) . . ?
C10 N2 C6 119.4(4) . . ?
C10 N2 Co1 128.7(3) . . ?
C6 N2 Co1 111.8(3) . . ?
C13 N3 C11 101.7(4) . . ?
C13 N4 C12 103.4(4) . . ?
C21 N5 C25 118.4(4) . . ?
C21 N5 Co1 129.5(3) . . ?
C25 N5 Co1 112.1(3) . . ?
C30 N6 C26 118.3(4) . . ?
C30 N6 Co1 129.1(3) . . ?
C26 N6 Co1 112.5(3) . . ?
C33 N7 C31 102.5(3) . . ?
C33 N8 C32 103.3(4) . . ?
C41 N9 C45 119.2(4) . . ?
C41 N9 Co1 128.6(3) . . ?
C45 N9 Co1 112.1(3) . . ?
C50 N10 C46 119.7(4) . . ?
C50 N10 Co1 129.1(3) . . ?
C46 N10 Co1 111.2(3) . . ?
C53 N11 C51 102.8(4) . . ?
C52 N12 C53 103.1(4) . . ?
N6 Co1 N10 177.62(15) . . ?
N6 Co1 N1 92.59(16) . . ?
N10 Co1 N1 89.76(16) . . ?
N6 Co1 N9 94.66(17) . . ?
N10 Co1 N9 84.83(17) . . ?
N1 Co1 N9 94.00(16) . . ?
N6 Co1 N5 84.23(15) . . ?
N10 Co1 N5 93.43(16) . . ?
N1 Co1 N5 176.03(14) . . ?
N9 Co1 N5 88.65(16) . . ?
N6 Co1 N2 87.16(17) . . ?
N10 Co1 N2 93.40(17) . . ?
N1 Co1 N2 84.48(15) . . ?
N9 Co1 N2 177.68(16) . . ?
N5 Co1 N2 92.96(16) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        73.58
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.064

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.020 0.750 380 119 ' '
2 0.750 0.057 0.250 380 119 ' '
3 0.356 0.064 0.973 6 1 ' '
4 0.856 0.435 0.473 6 1 ' '
5 0.144 0.564 0.527 6 0 ' '
6 0.644 0.936 0.027 6 0 ' '
_platon_squeeze_details          
;
The unit cell contains disordered solvent molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 801 A3 containing about 240 electrons which corresponds to approximately 2 ethanol molecules per formula unit. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
