# Electronic Supplementary Material (ESI) for ChemComm.
# 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).
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_rb17_68_1_250k
_database_code_depnum_ccdc_archive 'CCDC 1573880'
_audit_update_record             
;
2017-09-11 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7696(9)
_cell_length_b                   11.6828(8)
_cell_length_c                   11.8805(7)
_cell_angle_alpha                62.997(7)
_cell_angle_beta                 89.019(6)
_cell_angle_gamma                62.634(7)
_cell_volume                     1254.16(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    250(1)
_cell_measurement_reflns_used    2344
_cell_measurement_theta_min      3.8990
_cell_measurement_theta_max      30.0820

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.471
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.12799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30aa (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'XtaLAB Synergy R, EosS2'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 8.0388
_diffrn_reflns_number            4387
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0045
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.331
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measured_fraction_theta_full 0.827
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_Laue_measured_fraction_full 0.827
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_point_group_measured_fraction_full 0.827
_reflns_number_total             4129
_reflns_number_gt                3582
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.30aa (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30aa (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30aa (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1600P)²+1.3024P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4129
_refine_ls_number_parameters     300
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0827
_refine_ls_wR_factor_ref         0.2533
_refine_ls_wR_factor_gt          0.2379
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.0370(3) Uani 1 2 d S . P . .
N1 N 0.6294(3) -0.4320(3) 0.3158(3) 0.0391(8) Uani 1 1 d . . . . .
N2 N 0.5826(3) -0.2852(3) 0.2616(4) 0.0427(9) Uani 1 1 d . . . . .
N3 N 0.5600(3) -0.2313(3) 0.1351(3) 0.0410(8) Uani 1 1 d . . . . .
C1 C 0.6675(4) -0.5246(4) 0.4578(4) 0.0464(10) Uani 1 1 d . . . . .
H1A H 0.6794 -0.4705 0.4955 0.056 Uiso 1 1 calc R U . . .
H1B H 0.7523 -0.6158 0.4838 0.056 Uiso 1 1 calc R U . . .
C2 C 0.5662(4) -0.5664(4) 0.5122(5) 0.0470(11) Uani 1 1 d . . . . .
H2A H 0.5532 -0.6187 0.4730 0.056 Uiso 1 1 calc R U . . .
H2B H 0.6007 -0.6355 0.6063 0.056 Uiso 1 1 calc R U . . .
C4 C 0.5937(4) -0.3435(4) 0.1105(4) 0.0422(10) Uani 1 1 d . . . . .
H4 H 0.5874 -0.3336 0.0274 0.051 Uiso 1 1 calc R U . . .
C5 C 0.6382(4) -0.4737(4) 0.2260(4) 0.0416(10) Uani 1 1 d . . . . .
C6 C 0.6937(5) -0.6305(5) 0.2572(5) 0.0553(12) Uani 1 1 d . . . . .
H6A H 0.6532 -0.6765 0.3223 0.066 Uiso 1 1 calc R U . . .
H6B H 0.7886 -0.6859 0.2958 0.066 Uiso 1 1 calc R U . . .
C7 C 0.6724(6) -0.6446(6) 0.1414(6) 0.0674(15) Uani 1 1 d . . . . .
H7A H 0.5788 -0.6003 0.1086 0.101 Uiso 1 1 calc R U . . .
H7B H 0.7178 -0.7492 0.1665 0.101 Uiso 1 1 calc R U . . .
H7C H 0.7069 -0.5935 0.0739 0.101 Uiso 1 1 calc R U . . .
N11 N 0.1293(3) 0.2098(4) 0.0748(4) 0.0491(10) Uani 1 1 d . . . . .
N12 N 0.2112(3) 0.1898(4) -0.0015(4) 0.0460(9) Uani 1 1 d . . . . .
N13 N 0.3271(3) 0.0772(4) 0.0765(4) 0.0446(9) Uani 1 1 d . . . . .
C11 C -0.0095(4) 0.3317(5) 0.0176(6) 0.0622(14) Uani 1 1 d . . . . .
H11A H -0.0665 0.2929 0.0584 0.075 Uiso 1 1 calc R U . . .
H11B H -0.0313 0.3665 -0.0755 0.075 Uiso 1 1 calc R U . . .
C12 C -0.0379(4) 0.4621(5) 0.0343(6) 0.0583(13) Uani 1 1 d . . . . .
H12A H -0.0157 0.4272 0.1274 0.070 Uiso 1 1 calc R U . . .
H12B H -0.1325 0.5352 0.0004 0.070 Uiso 1 1 calc R U . . .
C14 C 0.3168(5) 0.0274(5) 0.1996(5) 0.0502(12) Uani 1 1 d . . . . .
H14 H 0.3856 -0.0525 0.2735 0.060 Uiso 1 1 calc R U . . .
C15 C 0.1886(5) 0.1125(5) 0.2002(5) 0.0506(12) Uani 1 1 d . . . . .
C16 C 0.1203(6) 0.1090(6) 0.3076(7) 0.0806(19) Uani 1 1 d . . . . .
H16A H 0.1257 0.1749 0.3340 0.097 Uiso 1 1 calc R U . . .
H16B H 0.0269 0.1485 0.2745 0.097 Uiso 1 1 calc R U . . .
C17 C 0.1744(8) -0.0389(7) 0.4214(7) 0.094(2) Uani 1 1 d . . . . .
H17A H 0.1675 -0.1045 0.3968 0.142 Uiso 1 1 calc R U . . .
H17B H 0.1255 -0.0328 0.4870 0.142 Uiso 1 1 calc R U . . .
H17C H 0.2664 -0.0780 0.4564 0.142 Uiso 1 1 calc R U . . .
N23 N 0.6060(4) 0.0014(4) 0.1472(4) 0.0513(10) Uani 1 1 d . . . . .
C23 C 0.6435(5) -0.0153(5) 0.2419(5) 0.0592(13) Uani 1 1 d . . . . .
C231 C 0.6915(10) -0.0378(9) 0.3664(7) 0.115(3) Uani 1 1 d . . . . .
H23A H 0.6218 0.0330 0.3850 0.173 Uiso 1 1 calc R U . . .
H23B H 0.7663 -0.0229 0.3628 0.173 Uiso 1 1 calc R U . . .
H23C H 0.7183 -0.1384 0.4346 0.173 Uiso 1 1 calc R U . . .
Cl1 Cl 0.34446(14) 0.34925(15) 0.28904(15) 0.0695(5) Uani 1 1 d . . . . .
O1 O 0.4488(7) 0.2527(8) 0.3988(7) 0.145(3) Uani 1 1 d . . . . .
O2 O 0.3772(12) 0.3180(15) 0.1919(10) 0.213(5) Uani 1 1 d . . . . .
O3 O 0.2388(9) 0.3443(16) 0.3109(11) 0.263(7) Uani 1 1 d . . . . .
O4 O 0.3327(15) 0.4825(9) 0.2483(12) 0.268(7) Uani 1 1 d . . . . .
C99 C 0.1330(12) 0.9305(15) -0.0561(12) 0.158(4) Uani 1 1 d D U . . .
N99 N 0.0445(16) 1.0183(17) -0.1535(13) 0.238(6) Uani 1 1 d D U . . .
C98 C 0.2195(9) 0.8328(10) 0.0785(9) 0.111(3) Uani 1 1 d D U . . .
H98A H 0.1658 0.8415 0.1403 0.167 Uiso 1 1 calc R U . . .
H98B H 0.2821 0.8633 0.0847 0.167 Uiso 1 1 calc R U . . .
H98C H 0.2669 0.7301 0.0980 0.167 Uiso 1 1 calc R U . . .
N88 N 0.9611(8) -0.6204(13) 0.3957(11) 0.140(3) Uani 1 1 d . U . . .
C89 C 0.9521(9) -0.5077(14) 0.3559(10) 0.111(3) Uani 1 1 d . U . . .
C88 C 0.9481(12) -0.3656(14) 0.3177(11) 0.153(4) Uani 1 1 d . U . . .
H88A H 0.9346 -0.3453 0.3890 0.230 Uiso 1 1 calc R U . . .
H88B H 0.8763 -0.2848 0.2416 0.230 Uiso 1 1 calc R U . . .
H88C H 1.0309 -0.3738 0.2977 0.230 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.174(3) 2_655 ?
Fe1 N3 2.174(3) . ?
Fe1 N23 2.176(4) 2_655 ?
Fe1 N23 2.176(4) . ?
Fe1 N13 2.185(4) . ?
Fe1 N13 2.185(4) 2_655 ?
N1 N2 1.342(4) . ?
N1 C5 1.344(6) . ?
N1 C1 1.463(5) . ?
N2 N3 1.314(5) . ?
N3 C4 1.352(5) . ?
C1 C2 1.518(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C2 1.517(8) 2_646 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C4 C5 1.366(6) . ?
C4 H4 0.9400 . ?
C5 C6 1.488(5) . ?
C6 C7 1.496(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
N11 N12 1.327(6) . ?
N11 C15 1.330(6) . ?
N11 C11 1.476(5) . ?
N12 N13 1.318(5) . ?
N13 C14 1.333(6) . ?
C11 C12 1.509(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C12 1.512(10) 2_565 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9400 . ?
C15 C16 1.491(8) . ?
C16 C17 1.455(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
N23 C23 1.113(6) . ?
C23 C231 1.455(8) . ?
C231 H23A 0.9700 . ?
C231 H23B 0.9700 . ?
C231 H23C 0.9700 . ?
Cl1 O3 1.288(8) . ?
Cl1 O4 1.340(8) . ?
Cl1 O2 1.360(8) . ?
Cl1 O1 1.388(6) . ?
C99 N99 1.207(9) . ?
C99 C98 1.492(9) . ?
C98 H98A 0.9700 . ?
C98 H98B 0.9700 . ?
C98 H98C 0.9700 . ?
N88 C89 1.129(13) . ?
C89 C88 1.488(16) . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
C88 H88C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N3 180.00(13) 2_655 . ?
N3 Fe1 N23 89.75(13) 2_655 2_655 ?
N3 Fe1 N23 90.25(13) . 2_655 ?
N3 Fe1 N23 90.25(13) 2_655 . ?
N3 Fe1 N23 89.75(13) . . ?
N23 Fe1 N23 180.0 2_655 . ?
N3 Fe1 N13 88.84(13) 2_655 . ?
N3 Fe1 N13 91.16(13) . . ?
N23 Fe1 N13 93.00(15) 2_655 . ?
N23 Fe1 N13 87.00(15) . . ?
N3 Fe1 N13 91.16(13) 2_655 2_655 ?
N3 Fe1 N13 88.84(13) . 2_655 ?
N23 Fe1 N13 87.00(15) 2_655 2_655 ?
N23 Fe1 N13 93.00(15) . 2_655 ?
N13 Fe1 N13 180.0 . 2_655 ?
N2 N1 C5 112.1(3) . . ?
N2 N1 C1 119.0(3) . . ?
C5 N1 C1 128.8(3) . . ?
N3 N2 N1 106.0(3) . . ?
N2 N3 C4 109.3(3) . . ?
N2 N3 Fe1 121.4(3) . . ?
C4 N3 Fe1 128.9(3) . . ?
N1 C1 C2 112.7(3) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 113.5(4) 2_646 . ?
C2 C2 H2A 108.9 2_646 . ?
C1 C2 H2A 108.9 . . ?
C2 C2 H2B 108.9 2_646 . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N3 C4 C5 108.9(4) . . ?
N3 C4 H4 125.6 . . ?
C5 C4 H4 125.6 . . ?
N1 C5 C4 103.7(3) . . ?
N1 C5 C6 124.2(4) . . ?
C4 C5 C6 132.0(4) . . ?
C5 C6 C7 113.6(4) . . ?
C5 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 N11 C15 112.2(4) . . ?
N12 N11 C11 120.2(4) . . ?
C15 N11 C11 127.6(4) . . ?
N13 N12 N11 106.3(3) . . ?
N12 N13 C14 109.2(4) . . ?
N12 N13 Fe1 121.4(3) . . ?
C14 N13 Fe1 129.4(3) . . ?
N11 C11 C12 113.1(4) . . ?
N11 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N11 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C12 113.3(5) . 2_565 ?
C11 C12 H12A 108.9 . . ?
C12 C12 H12A 108.9 2_565 . ?
C11 C12 H12B 108.9 . . ?
C12 C12 H12B 108.9 2_565 . ?
H12A C12 H12B 107.7 . . ?
N13 C14 C15 108.6(4) . . ?
N13 C14 H14 125.7 . . ?
C15 C14 H14 125.7 . . ?
N11 C15 C14 103.7(4) . . ?
N11 C15 C16 123.8(5) . . ?
C14 C15 C16 132.5(5) . . ?
C17 C16 C15 114.0(5) . . ?
C17 C16 H16A 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 161.7(4) . . ?
N23 C23 C231 179.3(7) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O3 Cl1 O4 114.8(10) . . ?
O3 Cl1 O2 108.2(9) . . ?
O4 Cl1 O2 105.9(8) . . ?
O3 Cl1 O1 113.1(6) . . ?
O4 Cl1 O1 104.0(7) . . ?
O2 Cl1 O1 110.7(7) . . ?
N99 C99 C98 167.6(16) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N88 C89 C88 173.8(11) . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.5(4) . . . . ?
C1 N1 N2 N3 178.4(3) . . . . ?
N1 N2 N3 C4 -0.7(4) . . . . ?
N1 N2 N3 Fe1 -174.2(2) . . . . ?
N2 N1 C1 C2 103.4(4) . . . . ?
C5 N1 C1 C2 -79.1(5) . . . . ?
N1 C1 C2 C2 -63.8(6) . . . 2_646 ?
N2 N3 C4 C5 0.6(5) . . . . ?
Fe1 N3 C4 C5 173.5(3) . . . . ?
N2 N1 C5 C4 -0.1(4) . . . . ?
C1 N1 C5 C4 -177.8(4) . . . . ?
N2 N1 C5 C6 176.4(4) . . . . ?
C1 N1 C5 C6 -1.2(7) . . . . ?
N3 C4 C5 N1 -0.3(4) . . . . ?
N3 C4 C5 C6 -176.5(4) . . . . ?
N1 C5 C6 C7 170.6(5) . . . . ?
C4 C5 C6 C7 -13.9(7) . . . . ?
C15 N11 N12 N13 -0.5(5) . . . . ?
C11 N11 N12 N13 178.2(4) . . . . ?
N11 N12 N13 C14 0.5(4) . . . . ?
N11 N12 N13 Fe1 -178.8(2) . . . . ?
N12 N11 C11 C12 -104.2(5) . . . . ?
C15 N11 C11 C12 74.2(6) . . . . ?
N11 C11 C12 C12 63.0(7) . . . 2_565 ?
N12 N13 C14 C15 -0.3(5) . . . . ?
Fe1 N13 C14 C15 178.9(3) . . . . ?
N12 N11 C15 C14 0.3(5) . . . . ?
C11 N11 C15 C14 -178.3(4) . . . . ?
N12 N11 C15 C16 -179.9(5) . . . . ?
C11 N11 C15 C16 1.5(7) . . . . ?
N13 C14 C15 N11 0.0(5) . . . . ?
N13 C14 C15 C16 -179.7(5) . . . . ?
N11 C15 C16 C17 149.5(6) . . . . ?
C14 C15 C16 C17 -30.9(10) . . . . ?

_refine_diff_density_max         1.430
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.093

####################################################################### 
# 
# 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_rb16_48_2_26_180k
_database_code_depnum_ccdc_archive 'CCDC 1573884'
_audit_update_record             
;
2017-09-11 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.799(2)
_cell_length_b                   11.225(2)
_cell_length_c                   11.573(2)
_cell_angle_alpha                64.323(19)
_cell_angle_beta                 83.075(16)
_cell_angle_gamma                62.158(19)
_cell_volume                     1215.1(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(1)
_cell_measurement_reflns_used    438
_cell_measurement_theta_min      3.4970
_cell_measurement_theta_max      19.9590

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.486
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            4903
_diffrn_reflns_av_unetI/netI     0.1167
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.432
_diffrn_reflns_theta_max         24.459
_diffrn_reflns_theta_full        24.459
_diffrn_measured_fraction_theta_max 0.697
_diffrn_measured_fraction_theta_full 0.697
_diffrn_reflns_Laue_measured_fraction_max 0.697
_diffrn_reflns_Laue_measured_fraction_full 0.697
_diffrn_reflns_point_group_measured_fraction_max 0.697
_diffrn_reflns_point_group_measured_fraction_full 0.697
_reflns_number_total             2804
_reflns_number_gt                1632
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1176P)²+1.8872P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2804
_refine_ls_number_parameters     300
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0810
_refine_ls_wR_factor_ref         0.2414
_refine_ls_wR_factor_gt          0.1925
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.0330(6) Uani 1 2 d S . P . .
N1 N 0.6231(6) -0.4157(7) 0.2925(6) 0.0317(17) Uani 1 1 d . U . . .
N2 N 0.5737(6) -0.2668(7) 0.2467(7) 0.0362(18) Uani 1 1 d . . . . .
N3 N 0.5513(6) -0.2144(7) 0.1201(7) 0.0327(17) Uani 1 1 d . . . . .
C1 C 0.6614(9) -0.5082(10) 0.4327(9) 0.048(2) Uani 1 1 d . . . . .
H1A H 0.6705 -0.4491 0.4709 0.057 Uiso 1 1 calc R U . . .
H1B H 0.7466 -0.5956 0.4462 0.057 Uiso 1 1 calc R U . . .
C2 C 0.5654(8) -0.5627(9) 0.5023(8) 0.040(2) Uani 1 1 d . . . . .
H2A H 0.5549 -0.6201 0.4629 0.048 Uiso 1 1 calc R U . . .
H2B H 0.6003 -0.6311 0.5935 0.048 Uiso 1 1 calc R U . . .
C4 C 0.5865(7) -0.3295(9) 0.0891(8) 0.031(2) Uani 1 1 d . . . . .
H4 H 0.5801 -0.3211 0.0046 0.037 Uiso 1 1 calc R U . . .
C5 C 0.6329(7) -0.4597(8) 0.1994(8) 0.033(2) Uani 1 1 d . . . . .
C6 C 0.6897(9) -0.6183(9) 0.2223(9) 0.046(2) Uani 1 1 d . . . . .
H6A H 0.6499 -0.6692 0.2939 0.055 Uiso 1 1 calc R U . . .
H6B H 0.7831 -0.6680 0.2487 0.055 Uiso 1 1 calc R U . . .
C7 C 0.6699(9) -0.6353(10) 0.1029(9) 0.051(3) Uani 1 1 d . . . . .
H7A H 0.5786 -0.6043 0.0863 0.077 Uiso 1 1 calc R U . . .
H7B H 0.7215 -0.7399 0.1178 0.077 Uiso 1 1 calc R U . . .
H7C H 0.6971 -0.5727 0.0283 0.077 Uiso 1 1 calc R U . . .
N11 N 0.1338(7) 0.2014(7) 0.0836(7) 0.0382(18) Uani 1 1 d . . . . .
N12 N 0.2254(6) 0.1738(7) 0.0023(7) 0.0348(18) Uani 1 1 d . . . . .
N13 N 0.3325(6) 0.0717(7) 0.0745(6) 0.0325(17) Uani 1 1 d . . . . .
C11 C 0.0005(8) 0.3141(9) 0.0336(9) 0.045(2) Uani 1 1 d . . . . .
H11A H -0.0575 0.2727 0.0825 0.053 Uiso 1 1 calc R U . . .
H11B H -0.0128 0.3357 -0.0576 0.053 Uiso 1 1 calc R U . . .
C12 C -0.0371(8) 0.4592(9) 0.0416(10) 0.048(3) Uani 1 1 d . . . . .
H12A H -0.0218 0.4376 0.1324 0.057 Uiso 1 1 calc R U . . .
H12B H -0.1305 0.5252 0.0143 0.057 Uiso 1 1 calc R U . . .
C14 C 0.3134(8) 0.0303(9) 0.2011(8) 0.037(2) Uani 1 1 d . . . . .
H14 H 0.3770 -0.0438 0.2720 0.044 Uiso 1 1 calc R U . . .
C15 C 0.1853(8) 0.1149(9) 0.2081(9) 0.037(2) Uani 1 1 d . . . . .
C16 C 0.1080(10) 0.1196(11) 0.3224(9) 0.058(3) Uani 1 1 d . . . . .
H16A H 0.0196 0.1417 0.3007 0.070 Uiso 1 1 calc R U . . .
H16B H 0.1017 0.2009 0.3406 0.070 Uiso 1 1 calc R U . . .
C17 C 0.1704(10) -0.0285(11) 0.4428(9) 0.060(3) Uani 1 1 d . . . . .
H17A H 0.1648 -0.1062 0.4296 0.090 Uiso 1 1 calc R U . . .
H17B H 0.1253 -0.0175 0.5172 0.090 Uiso 1 1 calc R U . . .
H17C H 0.2611 -0.0565 0.4585 0.090 Uiso 1 1 calc R U . . .
N23 N 0.5776(7) 0.0159(7) 0.1276(7) 0.0372(18) Uani 1 1 d . U . . .
C23 C 0.6149(9) 0.0179(9) 0.2135(9) 0.039(2) Uani 1 1 d . . . . .
C231 C 0.6612(10) 0.0190(11) 0.3234(9) 0.054(3) Uani 1 1 d . . . . .
H23A H 0.6065 0.1154 0.3262 0.080 Uiso 1 1 calc R U . . .
H23B H 0.7502 0.0037 0.3153 0.080 Uiso 1 1 calc R U . . .
H23C H 0.6583 -0.0611 0.4029 0.080 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3105(3) 0.3670(3) 0.2957(2) 0.0560(8) Uani 1 1 d . . . . .
O1 O 0.3248(17) 0.2691(19) 0.4153(11) 0.227(8) Uani 1 1 d . . . . .
O2 O 0.3486(16) 0.3072(15) 0.2115(12) 0.171(6) Uani 1 1 d . . . . .
O3 O 0.1888(11) 0.4690(16) 0.2615(19) 0.216(8) Uani 1 1 d . . . . .
O4 O 0.3880(10) 0.4364(15) 0.2816(11) 0.139(4) Uani 1 1 d . . . . .
C99 C 0.0612(14) -0.0826(15) 0.1546(13) 0.081(4) Uani 1 1 d . U . . .
C98 C 0.1907(11) -0.1838(13) 0.1414(12) 0.081(4) Uani 1 1 d . U . . .
H98A H 0.2516 -0.1507 0.1499 0.122 Uiso 1 1 calc R U . . .
H98B H 0.1927 -0.1839 0.0565 0.122 Uiso 1 1 calc R U . . .
H98C H 0.2151 -0.2848 0.2088 0.122 Uiso 1 1 calc R U . . .
N99 N -0.0417(13) -0.0041(13) 0.1669(12) 0.101(4) Uani 1 1 d . U . . .
C88 C 0.9006(11) -0.3330(13) 0.3301(11) 0.070(3) Uani 1 1 d . U . . .
H88A H 0.8182 -0.3250 0.3633 0.106 Uiso 1 1 calc R U . . .
H88B H 0.9539 -0.4330 0.3341 0.106 Uiso 1 1 calc R U . . .
H88C H 0.8849 -0.2583 0.2405 0.106 Uiso 1 1 calc R U . . .
C89 C 0.9664(12) -0.3074(13) 0.4070(12) 0.070(3) Uani 1 1 d . U . . .
N88 N 1.0172(10) -0.2887(13) 0.4720(12) 0.093(3) Uani 1 1 d . U . . .


_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 N23 1.938(9) . ?
Fe1 N23 1.938(9) 2_655 ?
Fe1 N13 2.000(6) . ?
Fe1 N13 2.000(6) 2_655 ?
Fe1 N3 2.008(6) . ?
Fe1 N3 2.008(6) 2_655 ?
N1 C5 1.340(10) . ?
N1 N2 1.345(9) . ?
N1 C1 1.482(11) . ?
N2 N3 1.328(9) . ?
N3 C4 1.354(10) . ?
C1 C2 1.519(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.514(16) 2_646 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C5 1.368(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.487(12) . ?
C6 C7 1.532(13) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N11 C15 1.355(11) . ?
N11 N12 1.358(9) . ?
N11 C11 1.461(10) . ?
N12 N13 1.297(9) . ?
N13 C14 1.357(10) . ?
C11 C12 1.517(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.522(17) 2_565 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.375(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.519(12) . ?
C16 C17 1.531(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N23 C23 1.148(11) . ?
C23 C231 1.451(14) . ?
C231 H23A 0.9800 . ?
C231 H23B 0.9800 . ?
C231 H23C 0.9800 . ?
Cl1 O1 1.310(10) . ?
Cl1 O3 1.319(11) . ?
Cl1 O2 1.335(11) . ?
Cl1 O4 1.410(10) . ?
C99 N99 1.157(15) . ?
C99 C98 1.457(17) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C88 C89 1.440(17) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 N88 1.154(15) . ?

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
N23 Fe1 N23 180.0 . 2_655 ?
N23 Fe1 N13 88.4(3) . . ?
N23 Fe1 N13 91.6(3) 2_655 . ?
N23 Fe1 N13 91.6(3) . 2_655 ?
N23 Fe1 N13 88.4(3) 2_655 2_655 ?
N13 Fe1 N13 180.0 . 2_655 ?
N23 Fe1 N3 89.6(3) . . ?
N23 Fe1 N3 90.4(3) 2_655 . ?
N13 Fe1 N3 92.4(3) . . ?
N13 Fe1 N3 87.6(3) 2_655 . ?
N23 Fe1 N3 90.4(3) . 2_655 ?
N23 Fe1 N3 89.6(3) 2_655 2_655 ?
N13 Fe1 N3 87.6(3) . 2_655 ?
N13 Fe1 N3 92.4(3) 2_655 2_655 ?
N3 Fe1 N3 180.0 . 2_655 ?
C5 N1 N2 112.7(6) . . ?
C5 N1 C1 128.7(7) . . ?
N2 N1 C1 118.6(7) . . ?
N3 N2 N1 105.3(6) . . ?
N2 N3 C4 109.4(6) . . ?
N2 N3 Fe1 122.1(5) . . ?
C4 N3 Fe1 127.9(6) . . ?
N1 C1 C2 113.0(7) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 113.1(9) 2_646 . ?
C2 C2 H2A 109.0 2_646 . ?
C1 C2 H2A 109.0 . . ?
C2 C2 H2B 109.0 2_646 . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N3 C4 C5 108.8(8) . . ?
N3 C4 H4 125.6 . . ?
C5 C4 H4 125.6 . . ?
N1 C5 C4 103.9(7) . . ?
N1 C5 C6 124.0(7) . . ?
C4 C5 C6 132.1(8) . . ?
C5 C6 C7 112.7(8) . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C15 N11 N12 110.8(6) . . ?
C15 N11 C11 128.3(7) . . ?
N12 N11 C11 120.8(7) . . ?
N13 N12 N11 106.4(6) . . ?
N12 N13 C14 110.7(7) . . ?
N12 N13 Fe1 122.0(5) . . ?
C14 N13 Fe1 127.3(5) . . ?
N11 C11 C12 114.0(8) . . ?
N11 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N11 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 C12 113.2(10) . 2_565 ?
C11 C12 H12A 108.9 . . ?
C12 C12 H12A 108.9 2_565 . ?
C11 C12 H12B 108.9 . . ?
C12 C12 H12B 108.9 2_565 . ?
H12A C12 H12B 107.8 . . ?
N13 C14 C15 107.6(7) . . ?
N13 C14 H14 126.2 . . ?
C15 C14 H14 126.2 . . ?
N11 C15 C14 104.5(7) . . ?
N11 C15 C16 123.8(8) . . ?
C14 C15 C16 131.7(8) . . ?
C15 C16 C17 111.5(8) . . ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 171.6(7) . . ?
N23 C23 C231 179.1(10) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O1 Cl1 O3 110.1(11) . . ?
O1 Cl1 O2 113.7(11) . . ?
O3 Cl1 O2 108.5(12) . . ?
O1 Cl1 O4 110.3(9) . . ?
O3 Cl1 O4 109.5(9) . . ?
O2 Cl1 O4 104.6(8) . . ?
N99 C99 C98 178.9(15) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
N88 C89 C88 177.8(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.0(9) . . . . ?
C1 N1 N2 N3 178.6(6) . . . . ?
N1 N2 N3 C4 0.0(8) . . . . ?
N1 N2 N3 Fe1 -171.3(4) . . . . ?
C5 N1 C1 C2 -78.1(11) . . . . ?
N2 N1 C1 C2 103.5(8) . . . . ?
N1 C1 C2 C2 -63.8(12) . . . 2_646 ?
N2 N3 C4 C5 0.0(9) . . . . ?
Fe1 N3 C4 C5 170.7(5) . . . . ?
N2 N1 C5 C4 0.0(9) . . . . ?
C1 N1 C5 C4 -178.5(7) . . . . ?
N2 N1 C5 C6 177.1(7) . . . . ?
C1 N1 C5 C6 -1.3(13) . . . . ?
N3 C4 C5 N1 0.0(8) . . . . ?
N3 C4 C5 C6 -176.8(8) . . . . ?
N1 C5 C6 C7 171.3(7) . . . . ?
C4 C5 C6 C7 -12.5(14) . . . . ?
C15 N11 N12 N13 0.1(8) . . . . ?
C11 N11 N12 N13 178.9(7) . . . . ?
N11 N12 N13 C14 0.7(8) . . . . ?
N11 N12 N13 Fe1 -176.4(5) . . . . ?
C15 N11 C11 C12 75.4(11) . . . . ?
N12 N11 C11 C12 -103.2(9) . . . . ?
N11 C11 C12 C12 64.3(13) . . . 2_565 ?
N12 N13 C14 C15 -1.1(9) . . . . ?
Fe1 N13 C14 C15 175.7(5) . . . . ?
N12 N11 C15 C14 -0.7(9) . . . . ?
C11 N11 C15 C14 -179.5(7) . . . . ?
N12 N11 C15 C16 179.7(8) . . . . ?
C11 N11 C15 C16 1.0(13) . . . . ?
N13 C14 C15 N11 1.1(9) . . . . ?
N13 C14 C15 C16 -179.4(9) . . . . ?
N11 C15 C16 C17 154.4(9) . . . . ?
C14 C15 C16 C17 -25.0(15) . . . . ?

_refine_diff_density_max         0.747
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_rb16_48_2_30_220k
_database_code_depnum_ccdc_archive 'CCDC 1573885'
_audit_update_record             
;
2017-09-11 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.706(2)
_cell_length_b                   11.680(2)
_cell_length_c                   11.898(2)
_cell_angle_alpha                63.100(19)
_cell_angle_beta                 89.376(16)
_cell_angle_gamma                62.860(18)
_cell_volume                     1251.2(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    220(1)
_cell_measurement_reflns_used    416
_cell_measurement_theta_min      3.6760
_cell_measurement_theta_max      18.0440

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.472
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            5086
_diffrn_reflns_av_unetI/netI     0.1440
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         24.495
_diffrn_reflns_theta_full        24.495
_diffrn_measured_fraction_theta_max 0.693
_diffrn_measured_fraction_theta_full 0.693
_diffrn_reflns_Laue_measured_fraction_max 0.693
_diffrn_reflns_Laue_measured_fraction_full 0.693
_diffrn_reflns_point_group_measured_fraction_max 0.693
_diffrn_reflns_point_group_measured_fraction_full 0.693
_reflns_number_total             2886
_reflns_number_gt                1461
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1742P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2886
_refine_ls_number_parameters     300
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1748
_refine_ls_R_factor_gt           0.0949
_refine_ls_wR_factor_ref         0.3115
_refine_ls_wR_factor_gt          0.2446
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.0479(8) Uani 1 2 d S . P . .
N1 N 0.6299(8) -0.4323(8) 0.3162(8) 0.045(2) Uani 1 1 d . U . . .
N2 N 0.5833(8) -0.2844(8) 0.2625(8) 0.046(2) Uani 1 1 d . . . . .
N3 N 0.5594(8) -0.2298(8) 0.1339(8) 0.049(2) Uani 1 1 d . . . . .
C1 C 0.6686(10) -0.5227(11) 0.4583(10) 0.055(3) Uani 1 1 d . . . . .
H1A H 0.6790 -0.4666 0.4946 0.066 Uiso 1 1 calc R U . . .
H1B H 0.7545 -0.6131 0.4853 0.066 Uiso 1 1 calc R U . . .
C2 C 0.5665(10) -0.5671(11) 0.5141(10) 0.055(3) Uani 1 1 d . . . . .
H2A H 0.5545 -0.6213 0.4764 0.066 Uiso 1 1 calc R U . . .
H2B H 0.6005 -0.6341 0.6084 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5915(9) -0.3406(11) 0.1086(9) 0.047(3) Uani 1 1 d . . . . .
H4 H 0.5848 -0.3305 0.0256 0.057 Uiso 1 1 calc R U . . .
C5 C 0.6358(10) -0.4712(11) 0.2253(10) 0.051(3) Uani 1 1 d . . . . .
C6 C 0.6951(12) -0.6303(11) 0.2576(11) 0.062(3) Uani 1 1 d . . . . .
H6A H 0.6565 -0.6782 0.3236 0.074 Uiso 1 1 calc R U . . .
H6B H 0.7906 -0.6832 0.2949 0.074 Uiso 1 1 calc R U . . .
C7 C 0.6726(13) -0.6443(13) 0.1407(11) 0.072(4) Uani 1 1 d . . . . .
H7A H 0.5789 -0.6045 0.1106 0.108 Uiso 1 1 calc R U . . .
H7B H 0.7215 -0.7483 0.1647 0.108 Uiso 1 1 calc R U . . .
H7C H 0.7031 -0.5890 0.0717 0.108 Uiso 1 1 calc R U . . .
N11 N 0.1257(9) 0.2117(10) 0.0716(10) 0.063(3) Uani 1 1 d . . . . .
N12 N 0.2118(9) 0.1903(10) -0.0037(9) 0.060(2) Uani 1 1 d . . . . .
N13 N 0.3260(8) 0.0776(9) 0.0745(8) 0.052(2) Uani 1 1 d . . . . .
C11 C -0.0120(10) 0.3346(12) 0.0110(12) 0.067(3) Uani 1 1 d . . . . .
H11A H -0.0716 0.2979 0.0482 0.081 Uiso 1 1 calc R U . . .
H11B H -0.0314 0.3704 -0.0824 0.081 Uiso 1 1 calc R U . . .
C12 C -0.0382(11) 0.4634(13) 0.0312(13) 0.076(4) Uani 1 1 d . . . . .
H12A H -0.1329 0.5378 -0.0034 0.091 Uiso 1 1 calc R U . . .
H12B H -0.0167 0.4262 0.1248 0.091 Uiso 1 1 calc R U . . .
C14 C 0.3160(11) 0.0247(11) 0.1995(11) 0.061(3) Uani 1 1 d . . . . .
H14 H 0.3844 -0.0575 0.2731 0.073 Uiso 1 1 calc R U . . .
C15 C 0.1866(12) 0.1136(12) 0.1998(12) 0.067(3) Uani 1 1 d . . . . .
C16 C 0.1145(14) 0.1085(13) 0.3056(12) 0.083(4) Uani 1 1 d . . . . .
H16A H 0.1151 0.1764 0.3321 0.099 Uiso 1 1 calc R U . . .
H16B H 0.0220 0.1438 0.2710 0.099 Uiso 1 1 calc R U . . .
C17 C 0.1723(15) -0.0405(14) 0.4199(12) 0.094(5) Uani 1 1 d . . . . .
H17A H 0.1643 -0.1063 0.3962 0.141 Uiso 1 1 calc R U . . .
H17B H 0.1258 -0.0357 0.4871 0.141 Uiso 1 1 calc R U . . .
H17C H 0.2651 -0.0784 0.4523 0.141 Uiso 1 1 calc R U . . .
N23 N 0.6066(9) -0.0015(9) 0.1497(10) 0.059(2) Uani 1 1 d . U . . .
C23 C 0.6423(13) -0.0156(13) 0.2450(12) 0.069(3) Uani 1 1 d . . . . .
C231 C 0.6902(17) -0.0382(17) 0.3673(14) 0.113(5) Uani 1 1 d . . . . .
H23A H 0.6500 0.0566 0.3646 0.169 Uiso 1 1 calc R U . . .
H23B H 0.7857 -0.0821 0.3852 0.169 Uiso 1 1 calc R U . . .
H23C H 0.6675 -0.1045 0.4354 0.169 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3469(4) 0.3478(4) 0.2907(3) 0.0749(11) Uani 1 1 d . . . . .
O1 O 0.4513(12) 0.2501(14) 0.4020(12) 0.141(4) Uani 1 1 d . . . . .
O2 O 0.3753(18) 0.319(2) 0.1918(14) 0.201(7) Uani 1 1 d . . . . .
O3 O 0.2375(16) 0.346(2) 0.3151(17) 0.239(10) Uani 1 1 d . . . . .
O4 O 0.333(2) 0.4820(16) 0.2486(17) 0.229(9) Uani 1 1 d . . . . .
C99 C 0.131(3) 0.936(3) -0.063(2) 0.223(12) Uani 1 1 d D U . . .
N99 N 0.043(2) 1.022(3) -0.157(2) 0.247(11) Uani 1 1 d D U . . .
C98 C 0.2102(17) 0.839(2) 0.0739(17) 0.124(6) Uani 1 1 d D U . . .
H98A H 0.1528 0.8555 0.1309 0.187 Uiso 1 1 calc R U . . .
H98B H 0.2778 0.8620 0.0836 0.187 Uiso 1 1 calc R U . . .
H98C H 0.2519 0.7353 0.0965 0.187 Uiso 1 1 calc R U . . .
N88 N 0.9632(19) -0.628(3) 0.402(2) 0.177(7) Uani 1 1 d . U . . .
C89 C 0.9516(19) -0.505(3) 0.356(2) 0.134(7) Uani 1 1 d . U . . .
C88 C 0.953(3) -0.361(3) 0.320(2) 0.194(10) Uani 1 1 d . U . . .
H88A H 0.9557 -0.3514 0.3966 0.291 Uiso 1 1 calc R U . . .
H88B H 0.8736 -0.2758 0.2533 0.291 Uiso 1 1 calc R U . . .
H88C H 1.0305 -0.3654 0.2877 0.291 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.163(8) . ?
Fe1 N3 2.163(8) 2_655 ?
Fe1 N23 2.175(11) . ?
Fe1 N23 2.176(11) 2_655 ?
Fe1 N13 2.182(8) 2_655 ?
Fe1 N13 2.182(8) . ?
N1 C5 1.340(12) . ?
N1 N2 1.356(10) . ?
N1 C1 1.465(12) . ?
N2 N3 1.338(11) . ?
N3 C4 1.346(12) . ?
C1 C2 1.541(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C2 1.517(19) 2_646 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C4 C5 1.379(13) . ?
C4 H4 0.9400 . ?
C5 C6 1.505(14) . ?
C6 C7 1.511(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
N11 N12 1.353(12) . ?
N11 C15 1.358(14) . ?
N11 C11 1.469(14) . ?
N12 N13 1.303(11) . ?
N13 C14 1.355(12) . ?
C11 C12 1.523(15) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C12 1.48(2) 2_565 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C14 C15 1.393(15) . ?
C14 H14 0.9400 . ?
C15 C16 1.502(15) . ?
C16 C17 1.463(17) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
N23 C23 1.125(13) . ?
C23 C231 1.427(18) . ?
C231 H23A 0.9700 . ?
C231 H23B 0.9700 . ?
C231 H23C 0.9700 . ?
Cl1 O3 1.315(14) . ?
Cl1 O4 1.341(14) . ?
Cl1 O2 1.360(12) . ?
Cl1 O1 1.394(12) . ?
C99 N99 1.177(10) . ?
C99 C98 1.482(10) . ?
C98 H98A 0.9700 . ?
C98 H98B 0.9700 . ?
C98 H98C 0.9700 . ?
N88 C89 1.22(3) . ?
C89 C88 1.55(3) . ?
C88 H88A 0.9700 . ?
C88 H88B 0.9700 . ?
C88 H88C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N3 180.0 . 2_655 ?
N3 Fe1 N23 89.0(3) . . ?
N3 Fe1 N23 91.0(3) 2_655 . ?
N3 Fe1 N23 91.0(3) . 2_655 ?
N3 Fe1 N23 89.0(3) 2_655 2_655 ?
N23 Fe1 N23 180.0 . 2_655 ?
N3 Fe1 N13 88.7(3) . 2_655 ?
N3 Fe1 N13 91.3(3) 2_655 2_655 ?
N23 Fe1 N13 93.0(3) . 2_655 ?
N23 Fe1 N13 87.0(3) 2_655 2_655 ?
N3 Fe1 N13 91.3(3) . . ?
N3 Fe1 N13 88.7(3) 2_655 . ?
N23 Fe1 N13 87.0(3) . . ?
N23 Fe1 N13 93.0(3) 2_655 . ?
N13 Fe1 N13 180.0 2_655 . ?
C5 N1 N2 111.8(8) . . ?
C5 N1 C1 130.7(8) . . ?
N2 N1 C1 117.5(8) . . ?
N3 N2 N1 105.4(7) . . ?
N2 N3 C4 109.7(8) . . ?
N2 N3 Fe1 121.2(6) . . ?
C4 N3 Fe1 128.7(6) . . ?
N1 C1 C2 112.5(9) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 112.2(10) 2_646 . ?
C2 C2 H2A 109.2 2_646 . ?
C1 C2 H2A 109.2 . . ?
C2 C2 H2B 109.2 2_646 . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N3 C4 C5 108.3(9) . . ?
N3 C4 H4 125.8 . . ?
C5 C4 H4 125.8 . . ?
N1 C5 C4 104.7(9) . . ?
N1 C5 C6 123.0(9) . . ?
C4 C5 C6 131.9(10) . . ?
C5 C6 C7 113.0(9) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 N11 C15 111.3(9) . . ?
N12 N11 C11 119.7(10) . . ?
C15 N11 C11 128.9(10) . . ?
N13 N12 N11 106.8(9) . . ?
N12 N13 C14 110.2(8) . . ?
N12 N13 Fe1 121.1(7) . . ?
C14 N13 Fe1 128.7(7) . . ?
N11 C11 C12 112.0(9) . . ?
N11 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
N11 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C12 C12 C11 114.1(12) 2_565 . ?
C12 C12 H12A 108.7 2_565 . ?
C11 C12 H12A 108.7 . . ?
C12 C12 H12B 108.7 2_565 . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
N13 C14 C15 108.1(10) . . ?
N13 C14 H14 126.0 . . ?
C15 C14 H14 126.0 . . ?
N11 C15 C14 103.6(9) . . ?
N11 C15 C16 123.0(11) . . ?
C14 C15 C16 133.2(12) . . ?
C17 C16 C15 113.2(10) . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16B 108.9 . . ?
C15 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 162.1(9) . . ?
N23 C23 C231 178.2(14) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O3 Cl1 O4 112.2(14) . . ?
O3 Cl1 O2 109.2(13) . . ?
O4 Cl1 O2 105.2(11) . . ?
O3 Cl1 O1 111.7(9) . . ?
O4 Cl1 O1 105.6(10) . . ?
O2 Cl1 O1 112.7(10) . . ?
N99 C99 C98 163(3) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N88 C89 C88 170(2) . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.0(10) . . . . ?
C1 N1 N2 N3 178.2(8) . . . . ?
N1 N2 N3 C4 -0.6(10) . . . . ?
N1 N2 N3 Fe1 -174.2(5) . . . . ?
C5 N1 C1 C2 -77.4(12) . . . . ?
N2 N1 C1 C2 104.8(10) . . . . ?
N1 C1 C2 C2 -63.6(14) . . . 2_646 ?
N2 N3 C4 C5 0.9(11) . . . . ?
Fe1 N3 C4 C5 174.0(6) . . . . ?
N2 N1 C5 C4 0.5(11) . . . . ?
C1 N1 C5 C4 -177.4(9) . . . . ?
N2 N1 C5 C6 174.4(9) . . . . ?
C1 N1 C5 C6 -3.5(16) . . . . ?
N3 C4 C5 N1 -0.9(11) . . . . ?
N3 C4 C5 C6 -174.0(11) . . . . ?
N1 C5 C6 C7 171.7(9) . . . . ?
C4 C5 C6 C7 -16.3(17) . . . . ?
C15 N11 N12 N13 1.6(11) . . . . ?
C11 N11 N12 N13 178.5(8) . . . . ?
N11 N12 N13 C14 0.1(11) . . . . ?
N11 N12 N13 Fe1 -179.1(6) . . . . ?
N12 N11 C11 C12 -104.7(11) . . . . ?
C15 N11 C11 C12 71.6(14) . . . . ?
N11 C11 C12 C12 63.9(17) . . . 2_565 ?
N12 N13 C14 C15 -1.7(12) . . . . ?
Fe1 N13 C14 C15 177.5(7) . . . . ?
N12 N11 C15 C14 -2.5(12) . . . . ?
C11 N11 C15 C14 -179.1(10) . . . . ?
N12 N11 C15 C16 -178.1(10) . . . . ?
C11 N11 C15 C16 5.3(18) . . . . ?
N13 C14 C15 N11 2.5(12) . . . . ?
N13 C14 C15 C16 177.5(12) . . . . ?
N11 C15 C16 C17 149.5(13) . . . . ?
C14 C15 C16 C17 -25(2) . . . . ?

_refine_diff_density_max         1.056
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_rb16_48_2_10_140K
_database_code_depnum_ccdc_archive 'CCDC 1573886'
_audit_update_record             
;
2017-09-11 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.760(3)
_cell_length_b                   11.193(3)
_cell_length_c                   11.526(3)
_cell_angle_alpha                64.44(2)
_cell_angle_beta                 83.26(2)
_cell_angle_gamma                62.29(3)
_cell_volume                     1205.0(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    430
_cell_measurement_theta_min      3.5140
_cell_measurement_theta_max      20.6940

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.490
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.53306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            4947
_diffrn_reflns_av_unetI/netI     0.1323
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.439
_diffrn_reflns_theta_max         24.569
_diffrn_reflns_theta_full        24.569
_diffrn_measured_fraction_theta_max 0.694
_diffrn_measured_fraction_theta_full 0.694
_diffrn_reflns_Laue_measured_fraction_max 0.694
_diffrn_reflns_Laue_measured_fraction_full 0.694
_diffrn_reflns_point_group_measured_fraction_max 0.694
_diffrn_reflns_point_group_measured_fraction_full 0.694
_reflns_number_total             2807
_reflns_number_gt                1539
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1445P)²+0.1180P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2807
_refine_ls_number_parameters     300
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.0878
_refine_ls_wR_factor_ref         0.2733
_refine_ls_wR_factor_gt          0.2163
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.0379(7) Uani 1 2 d S . P . .
N1 N 0.6232(7) -0.4155(8) 0.2925(7) 0.0339(18) Uani 1 1 d . . . . .
N2 N 0.5736(7) -0.2654(8) 0.2455(8) 0.041(2) Uani 1 1 d . . . . .
N3 N 0.5519(7) -0.2141(7) 0.1213(7) 0.0329(18) Uani 1 1 d . . . . .
C1 C 0.6625(9) -0.5083(11) 0.4317(9) 0.047(3) Uani 1 1 d . . . . .
H1A H 0.6730 -0.4499 0.4703 0.056 Uiso 1 1 calc R U . . .
H1B H 0.7474 -0.5959 0.4443 0.056 Uiso 1 1 calc R U . . .
C2 C 0.5656(9) -0.5632(10) 0.5029(9) 0.044(2) Uani 1 1 d . . . . .
H2A H 0.5552 -0.6218 0.4645 0.053 Uiso 1 1 calc R U . . .
H2B H 0.6006 -0.6304 0.5946 0.053 Uiso 1 1 calc R U . . .
C4 C 0.5863(9) -0.3284(10) 0.0869(10) 0.043(2) Uani 1 1 d . . . . .
H4 H 0.5791 -0.3192 0.0018 0.052 Uiso 1 1 calc R U . . .
C5 C 0.6335(8) -0.4595(10) 0.1990(9) 0.035(2) Uani 1 1 d . . . . .
C6 C 0.6926(10) -0.6206(10) 0.2225(10) 0.047(3) Uani 1 1 d . . . . .
H6A H 0.6553 -0.6733 0.2959 0.057 Uiso 1 1 calc R U . . .
H6B H 0.7868 -0.6686 0.2461 0.057 Uiso 1 1 calc R U . . .
C7 C 0.6687(10) -0.6357(11) 0.1022(10) 0.058(3) Uani 1 1 d . . . . .
H7A H 0.5770 -0.6064 0.0886 0.086 Uiso 1 1 calc R U . . .
H7B H 0.7209 -0.7396 0.1151 0.086 Uiso 1 1 calc R U . . .
H7C H 0.6929 -0.5707 0.0263 0.086 Uiso 1 1 calc R U . . .
N11 N 0.1324(8) 0.2012(8) 0.0843(8) 0.044(2) Uani 1 1 d . . . . .
N12 N 0.2237(8) 0.1752(8) 0.0021(8) 0.046(2) Uani 1 1 d . . . . .
N13 N 0.3330(7) 0.0704(8) 0.0744(8) 0.040(2) Uani 1 1 d . . . . .
C11 C 0.0002(9) 0.3127(11) 0.0328(11) 0.051(3) Uani 1 1 d . . . . .
H11A H -0.0584 0.2715 0.0807 0.061 Uiso 1 1 calc R U . . .
H11B H -0.0119 0.3340 -0.0589 0.061 Uiso 1 1 calc R U . . .
C12 C -0.0376(9) 0.4588(11) 0.0411(11) 0.052(3) Uani 1 1 d . . . . .
H12A H -0.0231 0.4371 0.1325 0.062 Uiso 1 1 calc R U . . .
H12B H -0.1310 0.5252 0.0130 0.062 Uiso 1 1 calc R U . . .
C14 C 0.3123(10) 0.0303(10) 0.2011(10) 0.044(2) Uani 1 1 d . . . . .
H14 H 0.3760 -0.0444 0.2723 0.053 Uiso 1 1 calc R U . . .
C15 C 0.1854(10) 0.1146(11) 0.2097(10) 0.046(3) Uani 1 1 d . . . . .
C16 C 0.1083(11) 0.1201(13) 0.3227(10) 0.062(3) Uani 1 1 d . . . . .
H16A H 0.0192 0.1441 0.2999 0.075 Uiso 1 1 calc R U . . .
H16B H 0.1034 0.2003 0.3420 0.075 Uiso 1 1 calc R U . . .
C17 C 0.1693(11) -0.0291(12) 0.4428(11) 0.062(3) Uani 1 1 d . . . . .
H17A H 0.1624 -0.1056 0.4283 0.093 Uiso 1 1 calc R U . . .
H17B H 0.1240 -0.0184 0.5175 0.093 Uiso 1 1 calc R U . . .
H17C H 0.2605 -0.0587 0.4595 0.093 Uiso 1 1 calc R U . . .
N23 N 0.5774(8) 0.0165(8) 0.1275(8) 0.042(2) Uani 1 1 d . . . . .
C23 C 0.6145(9) 0.0207(10) 0.2123(10) 0.042(2) Uani 1 1 d . . . . .
C231 C 0.6623(10) 0.0209(11) 0.3226(9) 0.052(3) Uani 1 1 d . . . . .
H23A H 0.6056 0.1152 0.3285 0.077 Uiso 1 1 calc R U . . .
H23B H 0.7500 0.0101 0.3120 0.077 Uiso 1 1 calc R U . . .
H23C H 0.6635 -0.0625 0.4018 0.077 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3102(3) 0.3689(3) 0.2947(3) 0.0570(9) Uani 1 1 d . . . . .
O1 O 0.3248(17) 0.2749(19) 0.4164(11) 0.185(7) Uani 1 1 d . . . . .
O2 O 0.3479(15) 0.3045(15) 0.2111(11) 0.145(5) Uani 1 1 d . . . . .
O3 O 0.1856(10) 0.4730(15) 0.2606(18) 0.178(7) Uani 1 1 d . . . . .
O4 O 0.3880(10) 0.4421(14) 0.2797(11) 0.120(4) Uani 1 1 d . . . . .
C99 C 0.0583(14) -0.0812(15) 0.1562(13) 0.075(4) Uani 1 1 d . U . . .
C98 C 0.1877(12) -0.1848(14) 0.1458(13) 0.078(4) Uani 1 1 d . U . . .
H98A H 0.2512 -0.1731 0.1821 0.117 Uiso 1 1 calc R U . . .
H98B H 0.1991 -0.1637 0.0547 0.117 Uiso 1 1 calc R U . . .
H98C H 0.2001 -0.2873 0.1938 0.117 Uiso 1 1 calc R U . . .
N99 N -0.0436(13) -0.0020(14) 0.1663(12) 0.092(3) Uani 1 1 d . U . . .
C88 C 0.8978(12) -0.3304(14) 0.3299(12) 0.076(4) Uani 1 1 d . U . . .
H88A H 0.8169 -0.3262 0.3657 0.114 Uiso 1 1 calc R U . . .
H88B H 0.9518 -0.4285 0.3300 0.114 Uiso 1 1 calc R U . . .
H88C H 0.8786 -0.2525 0.2411 0.114 Uiso 1 1 calc R U . . .
C89 C 0.9659(11) -0.3066(13) 0.4082(13) 0.064(3) Uani 1 1 d . U . . .
N88 N 1.0184(10) -0.2887(13) 0.4719(12) 0.084(3) Uani 1 1 d . U . . .


_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 N23 1.931(10) . ?
Fe1 N23 1.931(10) 2_655 ?
Fe1 N13 1.990(7) . ?
Fe1 N13 1.990(7) 2_655 ?
Fe1 N3 2.005(7) . ?
Fe1 N3 2.005(7) 2_655 ?
N1 C5 1.339(11) . ?
N1 N2 1.354(10) . ?
N1 C1 1.468(12) . ?
N2 N3 1.299(10) . ?
N3 C4 1.370(11) . ?
C1 C2 1.531(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.516(18) 2_646 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C5 1.381(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.505(13) . ?
C6 C7 1.539(14) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N11 N12 1.358(10) . ?
N11 C15 1.364(12) . ?
N11 C11 1.449(12) . ?
N12 N13 1.314(10) . ?
N13 C14 1.359(12) . ?
C11 C12 1.527(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.529(18) 2_565 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.365(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.504(14) . ?
C16 C17 1.531(15) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N23 C23 1.142(12) . ?
C23 C231 1.450(15) . ?
C231 H23A 0.9800 . ?
C231 H23B 0.9800 . ?
C231 H23C 0.9800 . ?
Cl1 O1 1.311(11) . ?
Cl1 O3 1.345(11) . ?
Cl1 O2 1.359(10) . ?
Cl1 O4 1.442(10) . ?
C99 N99 1.142(15) . ?
C99 C98 1.452(18) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C88 C89 1.450(18) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 N88 1.144(15) . ?

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
N23 Fe1 N23 180.0(4) . 2_655 ?
N23 Fe1 N13 88.5(3) . . ?
N23 Fe1 N13 91.5(3) 2_655 . ?
N23 Fe1 N13 91.5(3) . 2_655 ?
N23 Fe1 N13 88.5(3) 2_655 2_655 ?
N13 Fe1 N13 180.0 . 2_655 ?
N23 Fe1 N3 89.3(3) . . ?
N23 Fe1 N3 90.7(3) 2_655 . ?
N13 Fe1 N3 92.1(3) . . ?
N13 Fe1 N3 87.9(3) 2_655 . ?
N23 Fe1 N3 90.7(3) . 2_655 ?
N23 Fe1 N3 89.3(3) 2_655 2_655 ?
N13 Fe1 N3 87.9(3) . 2_655 ?
N13 Fe1 N3 92.1(3) 2_655 2_655 ?
N3 Fe1 N3 180.0 . 2_655 ?
C5 N1 N2 112.3(7) . . ?
C5 N1 C1 128.3(7) . . ?
N2 N1 C1 119.4(7) . . ?
N3 N2 N1 105.7(6) . . ?
N2 N3 C4 110.6(7) . . ?
N2 N3 Fe1 122.6(5) . . ?
C4 N3 Fe1 126.2(6) . . ?
N1 C1 C2 113.2(8) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 112.9(10) 2_646 . ?
C2 C2 H2A 109.0 2_646 . ?
C1 C2 H2A 109.0 . . ?
C2 C2 H2B 109.0 2_646 . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N3 C4 C5 107.1(8) . . ?
N3 C4 H4 126.4 . . ?
C5 C4 H4 126.4 . . ?
N1 C5 C4 104.3(7) . . ?
N1 C5 C6 123.7(8) . . ?
C4 C5 C6 131.9(9) . . ?
C5 C6 C7 111.6(8) . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 N11 C15 110.8(7) . . ?
N12 N11 C11 119.7(8) . . ?
C15 N11 C11 129.4(8) . . ?
N13 N12 N11 106.6(8) . . ?
N12 N13 C14 109.4(8) . . ?
N12 N13 Fe1 122.5(6) . . ?
C14 N13 Fe1 128.0(7) . . ?
N11 C11 C12 113.5(8) . . ?
N11 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
N11 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 C12 113.5(10) . 2_565 ?
C11 C12 H12A 108.9 . . ?
C12 C12 H12A 108.9 2_565 . ?
C11 C12 H12B 108.9 . . ?
C12 C12 H12B 108.9 2_565 . ?
H12A C12 H12B 107.7 . . ?
N13 C14 C15 109.1(9) . . ?
N13 C14 H14 125.5 . . ?
C15 C14 H14 125.5 . . ?
N11 C15 C14 104.1(8) . . ?
N11 C15 C16 123.1(9) . . ?
C14 C15 C16 132.8(10) . . ?
C15 C16 C17 111.3(9) . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 172.3(8) . . ?
N23 C23 C231 178.1(10) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O1 Cl1 O3 109.4(11) . . ?
O1 Cl1 O2 114.4(10) . . ?
O3 Cl1 O2 109.0(10) . . ?
O1 Cl1 O4 108.8(8) . . ?
O3 Cl1 O4 108.6(8) . . ?
O2 Cl1 O4 106.4(8) . . ?
N99 C99 C98 178.7(15) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
N88 C89 C88 178.7(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.2(9) . . . . ?
C1 N1 N2 N3 178.1(7) . . . . ?
N1 N2 N3 C4 0.1(9) . . . . ?
N1 N2 N3 Fe1 -171.6(5) . . . . ?
C5 N1 C1 C2 -79.4(11) . . . . ?
N2 N1 C1 C2 103.2(9) . . . . ?
N1 C1 C2 C2 -62.6(13) . . . 2_646 ?
N2 N3 C4 C5 -0.5(10) . . . . ?
Fe1 N3 C4 C5 171.0(6) . . . . ?
N2 N1 C5 C4 -0.5(9) . . . . ?
C1 N1 C5 C4 -178.1(8) . . . . ?
N2 N1 C5 C6 176.3(8) . . . . ?
C1 N1 C5 C6 -1.3(14) . . . . ?
N3 C4 C5 N1 0.6(9) . . . . ?
N3 C4 C5 C6 -175.9(9) . . . . ?
N1 C5 C6 C7 169.6(8) . . . . ?
C4 C5 C6 C7 -14.5(14) . . . . ?
C15 N11 N12 N13 1.7(9) . . . . ?
C11 N11 N12 N13 179.9(7) . . . . ?
N11 N12 N13 C14 -0.4(9) . . . . ?
N11 N12 N13 Fe1 -176.2(5) . . . . ?
N12 N11 C11 C12 -103.2(10) . . . . ?
C15 N11 C11 C12 74.6(12) . . . . ?
N11 C11 C12 C12 64.5(15) . . . 2_565 ?
N12 N13 C14 C15 -1.0(10) . . . . ?
Fe1 N13 C14 C15 174.6(6) . . . . ?
N12 N11 C15 C14 -2.2(10) . . . . ?
C11 N11 C15 C14 179.8(8) . . . . ?
N12 N11 C15 C16 179.3(8) . . . . ?
C11 N11 C15 C16 1.3(15) . . . . ?
N13 C14 C15 N11 1.9(10) . . . . ?
N13 C14 C15 C16 -179.7(10) . . . . ?
N11 C15 C16 C17 152.7(9) . . . . ?
C14 C15 C16 C17 -25.3(16) . . . . ?

_refine_diff_density_max         0.804
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.096

####################################################################### 
# 
# 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_rb17_1a_12_130k
_database_code_depnum_ccdc_archive 'CCDC 1573881'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4674(7)
_cell_length_b                   11.6318(7)
_cell_length_c                   11.8386(7)
_cell_angle_alpha                63.371(6)
_cell_angle_beta                 90.780(5)
_cell_angle_gamma                63.371(6)
_cell_volume                     1215.56(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(1)
_cell_measurement_reflns_used    2766
_cell_measurement_theta_min      3.9260
_cell_measurement_theta_max      30.2840

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.486
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.31102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30aa (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'XtaLAB Synergy R, EosS2'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 8.0388
_diffrn_reflns_number            4202
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0053
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.371
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measured_fraction_theta_full 0.820
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_Laue_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_point_group_measured_fraction_full 0.820
_reflns_number_total             3958
_reflns_number_gt                3617
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.30aa (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30aa (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30aa (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0667P)²+1.5634P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3958
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.01917(19) Uani 1 2 d S . P . .
N1 N 0.6316(2) -0.4300(2) 0.3186(3) 0.0211(6) Uani 1 1 d . . . . .
N2 N 0.5853(2) -0.2834(3) 0.2635(3) 0.0238(6) Uani 1 1 d . . . . .
N3 N 0.5615(2) -0.2292(3) 0.1356(3) 0.0228(6) Uani 1 1 d . . . . .
C1 C 0.6716(3) -0.5227(3) 0.4620(3) 0.0249(7) Uani 1 1 d . . . . .
H1A H 0.6831 -0.4672 0.5006 0.030 Uiso 1 1 calc R U . . .
H1B H 0.7601 -0.6143 0.4902 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5687(3) -0.5667(3) 0.5147(3) 0.0249(7) Uani 1 1 d . . . . .
H2A H 0.6046 -0.6353 0.6108 0.030 Uiso 1 1 calc R U . . .
H2B H 0.5568 -0.6215 0.4755 0.030 Uiso 1 1 calc R U . . .
C4 C 0.5941(3) -0.3414(3) 0.1100(3) 0.0225(7) Uani 1 1 d . . . . .
H4 H 0.5866 -0.3314 0.0257 0.027 Uiso 1 1 calc R U . . .
C5 C 0.6397(3) -0.4718(3) 0.2279(3) 0.0234(7) Uani 1 1 d . . . . .
C6 C 0.6954(3) -0.6294(3) 0.2607(3) 0.0301(8) Uani 1 1 d . . . . .
H6A H 0.6541 -0.6755 0.3263 0.036 Uiso 1 1 calc R U . . .
H6B H 0.7943 -0.6861 0.3009 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6694(4) -0.6421(4) 0.1419(4) 0.0373(9) Uani 1 1 d . . . . .
H7A H 0.5720 -0.5984 0.1089 0.056 Uiso 1 1 calc R U . . .
H7B H 0.7170 -0.7475 0.1668 0.056 Uiso 1 1 calc R U . . .
H7C H 0.7026 -0.5885 0.0732 0.056 Uiso 1 1 calc R U . . .
N11 N 0.1236(2) 0.2133(3) 0.0706(3) 0.0230(6) Uani 1 1 d . . . . .
N12 N 0.2076(2) 0.1919(3) -0.0045(3) 0.0245(6) Uani 1 1 d . . . . .
N13 N 0.3263(2) 0.0773(3) 0.0768(3) 0.0239(6) Uani 1 1 d . . . . .
C11 C -0.0179(3) 0.3379(3) 0.0096(3) 0.0279(8) Uani 1 1 d . . . . .
H11A H -0.0788 0.3006 0.0471 0.034 Uiso 1 1 calc R U . . .
H11B H -0.0403 0.3753 -0.0857 0.034 Uiso 1 1 calc R U . . .
C12 C -0.0431(3) 0.4661(3) 0.0305(3) 0.0262(7) Uani 1 1 d . . . . .
H12A H -0.0224 0.4293 0.1257 0.031 Uiso 1 1 calc R U . . .
H12B H -0.1401 0.5444 -0.0089 0.031 Uiso 1 1 calc R U . . .
C14 C 0.3165(3) 0.0271(3) 0.2018(3) 0.0248(8) Uani 1 1 d . . . . .
H14 H 0.3881 -0.0545 0.2781 0.030 Uiso 1 1 calc R U . . .
C15 C 0.1860(3) 0.1139(3) 0.2000(3) 0.0230(7) Uani 1 1 d . . . . .
C16 C 0.1157(3) 0.1116(3) 0.3057(4) 0.0330(9) Uani 1 1 d . . . . .
H16A H 0.0179 0.1558 0.2692 0.040 Uiso 1 1 calc R U . . .
H16B H 0.1257 0.1737 0.3366 0.040 Uiso 1 1 calc R U . . .
C17 C 0.1718(4) -0.0451(4) 0.4209(4) 0.0359(8) Uani 1 1 d . . . . .
H17A H 0.1572 -0.1055 0.3917 0.054 Uiso 1 1 calc R U . . .
H17B H 0.1255 -0.0412 0.4891 0.054 Uiso 1 1 calc R U . . .
H17C H 0.2690 -0.0901 0.4563 0.054 Uiso 1 1 calc R U . . .
N23 N 0.6131(3) -0.0026(3) 0.1493(3) 0.0271(6) Uani 1 1 d . . . . .
C23 C 0.6537(3) -0.0245(3) 0.2492(4) 0.0296(8) Uani 1 1 d . . . . .
C231 C 0.7044(4) -0.0539(5) 0.3779(4) 0.0508(11) Uani 1 1 d . . . . .
H23A H 0.6462 0.0324 0.3868 0.076 Uiso 1 1 calc R U . . .
H23B H 0.7970 -0.0719 0.3883 0.076 Uiso 1 1 calc R U . . .
H23C H 0.7043 -0.1422 0.4456 0.076 Uiso 1 1 calc R U . . .
Cl1 Cl 0.35953(8) 0.33820(8) 0.29065(8) 0.0315(2) Uani 1 1 d . . . . .
O1 O 0.4632(3) 0.2334(3) 0.4118(3) 0.0515(7) Uani 1 1 d . . . . .
O2 O 0.4005(3) 0.2946(4) 0.1969(3) 0.0606(9) Uani 1 1 d . . . . .
O3 O 0.2363(3) 0.3414(4) 0.3076(3) 0.0633(9) Uani 1 1 d . . . . .
O4 O 0.3429(4) 0.4820(3) 0.2473(3) 0.0695(10) Uani 1 1 d . . . . .
C99 C 0.1299(4) 0.9301(4) -0.0598(5) 0.0459(10) Uani 1 1 d . . . . .
N99 N 0.0543(4) 1.0045(5) -0.1633(5) 0.0638(11) Uani 1 1 d . . . . .
C98 C 0.2237(4) 0.8356(4) 0.0695(4) 0.0462(10) Uani 1 1 d . . . . .
H98A H 0.1739 0.8453 0.1344 0.069 Uiso 1 1 calc R U . . .
H98B H 0.2904 0.8661 0.0710 0.069 Uiso 1 1 calc R U . . .
H98C H 0.2703 0.7314 0.0907 0.069 Uiso 1 1 calc R U . . .
N88 N 0.9509(4) -0.5790(5) 0.3747(4) 0.0597(11) Uani 1 1 d . . . . .
C89 C 0.9649(4) -0.4791(6) 0.3451(4) 0.0493(11) Uani 1 1 d . . . . .
C88 C 0.9859(5) -0.3544(5) 0.3083(4) 0.0619(13) Uani 1 1 d . . . . .
H88A H 0.9732 -0.3270 0.3762 0.093 Uiso 1 1 calc R U . . .
H88B H 0.9206 -0.2690 0.2246 0.093 Uiso 1 1 calc R U . . .
H88C H 1.0781 -0.3829 0.2993 0.093 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.152(2) . ?
Fe1 N3 2.152(2) 2_655 ?
Fe1 N23 2.159(3) 2_655 ?
Fe1 N23 2.159(3) . ?
Fe1 N13 2.186(3) . ?
Fe1 N13 2.186(3) 2_655 ?
N1 N2 1.340(3) . ?
N1 C5 1.352(4) . ?
N1 C1 1.467(4) . ?
N2 N3 1.320(4) . ?
N3 C4 1.361(4) . ?
C1 C2 1.522(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.524(6) 2_646 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C5 1.376(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.491(4) . ?
C6 C7 1.518(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N11 N12 1.337(4) . ?
N11 C15 1.355(4) . ?
N11 C11 1.475(3) . ?
N12 N13 1.321(3) . ?
N13 C14 1.353(4) . ?
C11 C12 1.521(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.527(6) 2_565 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.373(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.494(5) . ?
C16 C17 1.514(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N23 C23 1.136(4) . ?
C23 C231 1.451(5) . ?
C231 H23A 0.9800 . ?
C231 H23B 0.9800 . ?
C231 H23C 0.9800 . ?
Cl1 O3 1.417(3) . ?
Cl1 O2 1.420(3) . ?
Cl1 O4 1.428(3) . ?
Cl1 O1 1.429(3) . ?
C99 N99 1.161(6) . ?
C99 C98 1.448(6) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
N88 C89 1.142(6) . ?
C89 C88 1.449(7) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N3 180.0 . 2_655 ?
N3 Fe1 N23 91.15(9) . 2_655 ?
N3 Fe1 N23 88.85(9) 2_655 2_655 ?
N3 Fe1 N23 88.85(9) . . ?
N3 Fe1 N23 91.15(9) 2_655 . ?
N23 Fe1 N23 180.0 2_655 . ?
N3 Fe1 N13 90.99(9) . . ?
N3 Fe1 N13 89.01(9) 2_655 . ?
N23 Fe1 N13 93.37(10) 2_655 . ?
N23 Fe1 N13 86.63(10) . . ?
N3 Fe1 N13 89.01(9) . 2_655 ?
N3 Fe1 N13 90.99(9) 2_655 2_655 ?
N23 Fe1 N13 86.63(10) 2_655 2_655 ?
N23 Fe1 N13 93.37(10) . 2_655 ?
N13 Fe1 N13 180.0 . 2_655 ?
N2 N1 C5 112.0(2) . . ?
N2 N1 C1 119.0(2) . . ?
C5 N1 C1 129.0(2) . . ?
N3 N2 N1 106.2(2) . . ?
N2 N3 C4 109.7(2) . . ?
N2 N3 Fe1 121.73(18) . . ?
C4 N3 Fe1 128.3(2) . . ?
N1 C1 C2 112.9(2) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 C2 113.1(3) . 2_646 ?
C1 C2 H2A 109.0 . . ?
C2 C2 H2A 109.0 2_646 . ?
C1 C2 H2B 109.0 . . ?
C2 C2 H2B 109.0 2_646 . ?
H2A C2 H2B 107.8 . . ?
N3 C4 C5 108.0(3) . . ?
N3 C4 H4 126.0 . . ?
C5 C4 H4 126.0 . . ?
N1 C5 C4 104.2(2) . . ?
N1 C5 C6 123.9(3) . . ?
C4 C5 C6 131.8(3) . . ?
C5 C6 C7 112.9(3) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 N11 C15 112.2(2) . . ?
N12 N11 C11 119.8(3) . . ?
C15 N11 C11 127.9(3) . . ?
N13 N12 N11 106.0(2) . . ?
N12 N13 C14 109.6(3) . . ?
N12 N13 Fe1 120.0(2) . . ?
C14 N13 Fe1 130.46(19) . . ?
N11 C11 C12 112.5(2) . . ?
N11 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N11 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C12 112.0(3) . 2_565 ?
C11 C12 H12A 109.2 . . ?
C12 C12 H12A 109.2 2_565 . ?
C11 C12 H12B 109.2 . . ?
C12 C12 H12B 109.2 2_565 . ?
H12A C12 H12B 107.9 . . ?
N13 C14 C15 108.6(3) . . ?
N13 C14 H14 125.7 . . ?
C15 C14 H14 125.7 . . ?
N11 C15 C14 103.6(3) . . ?
N11 C15 C16 123.5(3) . . ?
C14 C15 C16 132.9(3) . . ?
C15 C16 C17 112.2(3) . . ?
C15 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 159.6(3) . . ?
N23 C23 C231 179.0(4) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O3 Cl1 O2 109.2(2) . . ?
O3 Cl1 O4 110.3(2) . . ?
O2 Cl1 O4 109.9(2) . . ?
O3 Cl1 O1 110.4(2) . . ?
O2 Cl1 O1 108.78(19) . . ?
O4 Cl1 O1 108.21(19) . . ?
N99 C99 C98 179.2(4) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N88 C89 C88 178.7(4) . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.8(3) . . . . ?
C1 N1 N2 N3 178.1(2) . . . . ?
N1 N2 N3 C4 -0.7(3) . . . . ?
N1 N2 N3 Fe1 -175.03(17) . . . . ?
N2 N1 C1 C2 105.1(3) . . . . ?
C5 N1 C1 C2 -78.1(4) . . . . ?
N1 C1 C2 C2 -63.1(4) . . . 2_646 ?
N2 N3 C4 C5 0.4(3) . . . . ?
Fe1 N3 C4 C5 174.25(19) . . . . ?
N2 N1 C5 C4 -0.5(3) . . . . ?
C1 N1 C5 C4 -177.5(3) . . . . ?
N2 N1 C5 C6 176.2(3) . . . . ?
C1 N1 C5 C6 -0.7(5) . . . . ?
N3 C4 C5 N1 0.1(3) . . . . ?
N3 C4 C5 C6 -176.3(3) . . . . ?
N1 C5 C6 C7 169.6(3) . . . . ?
C4 C5 C6 C7 -14.7(5) . . . . ?
C15 N11 N12 N13 -0.1(3) . . . . ?
C11 N11 N12 N13 178.0(2) . . . . ?
N11 N12 N13 C14 0.1(3) . . . . ?
N11 N12 N13 Fe1 -179.19(16) . . . . ?
N12 N11 C11 C12 -105.5(3) . . . . ?
C15 N11 C11 C12 72.2(4) . . . . ?
N11 C11 C12 C12 61.3(4) . . . 2_565 ?
N12 N13 C14 C15 -0.2(3) . . . . ?
Fe1 N13 C14 C15 179.08(19) . . . . ?
N12 N11 C15 C14 0.0(3) . . . . ?
C11 N11 C15 C14 -177.9(3) . . . . ?
N12 N11 C15 C16 -179.5(3) . . . . ?
C11 N11 C15 C16 2.7(4) . . . . ?
N13 C14 C15 N11 0.1(3) . . . . ?
N13 C14 C15 C16 179.5(3) . . . . ?
N11 C15 C16 C17 146.9(3) . . . . ?
C14 C15 C16 C17 -32.4(5) . . . . ?

_refine_diff_density_max         0.607
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_rb16_48_3_80k
_database_code_depnum_ccdc_archive 'CCDC 1573882'
_audit_update_record             
;
2017-09-11 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5506(5)
_cell_length_b                   11.5833(5)
_cell_length_c                   11.6586(5)
_cell_angle_alpha                62.604(4)
_cell_angle_beta                 88.651(3)
_cell_angle_gamma                62.157(4)
_cell_volume                     1187.64(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    80(1)
_cell_measurement_reflns_used    4092
_cell_measurement_theta_min      3.5120
_cell_measurement_theta_max      34.9430

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.498
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      80(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            9718
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.222
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4842
_reflns_number_gt                3953
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0811P)²+1.8800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4842
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1732
_refine_ls_wR_factor_gt          0.1602
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.01994(19) Uani 1 2 d S . P . .
N1 N 0.6302(3) -0.4238(3) 0.3111(2) 0.0209(5) Uani 1 1 d . . . . .
N2 N 0.5824(3) -0.2753(3) 0.2573(2) 0.0221(5) Uani 1 1 d . . . . .
N3 N 0.5582(3) -0.2177(3) 0.1268(2) 0.0226(5) Uani 1 1 d . . . . .
C1 C 0.6706(3) -0.5209(3) 0.4572(3) 0.0239(6) Uani 1 1 d . . . . .
H1A H 0.6815 -0.4662 0.4970 0.029 Uiso 1 1 calc R U . . .
H1B H 0.7592 -0.6134 0.4830 0.029 Uiso 1 1 calc R U . . .
C2 C 0.5687(3) -0.5670(3) 0.5137(3) 0.0236(6) Uani 1 1 d . . . . .
H2A H 0.5586 -0.6226 0.4746 0.028 Uiso 1 1 calc R U . . .
H2B H 0.6042 -0.6368 0.6112 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5911(3) -0.3299(3) 0.0993(3) 0.0223(6) Uani 1 1 d . . . . .
H4 H 0.5828 -0.3178 0.0130 0.027 Uiso 1 1 calc R U . . .
C5 C 0.6385(3) -0.4636(3) 0.2178(3) 0.0225(6) Uani 1 1 d . . . . .
C6 C 0.6970(4) -0.6235(4) 0.2500(3) 0.0294(7) Uani 1 1 d . . . . .
H6A H 0.6591 -0.6730 0.3205 0.035 Uiso 1 1 calc R U . . .
H6B H 0.7959 -0.6791 0.2855 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6692(4) -0.6354(4) 0.1305(4) 0.0356(8) Uani 1 1 d . . . . .
H7A H 0.5725 -0.5957 0.1039 0.053 Uiso 1 1 calc R U . . .
H7B H 0.7204 -0.7418 0.1541 0.053 Uiso 1 1 calc R U . . .
H7C H 0.6966 -0.5763 0.0565 0.053 Uiso 1 1 calc R U . . .
N11 N 0.1323(3) 0.2095(3) 0.0698(3) 0.0289(6) Uani 1 1 d . . . . .
N12 N 0.2171(3) 0.1861(3) -0.0083(3) 0.0264(6) Uani 1 1 d . . . . .
N13 N 0.3360(3) 0.0735(3) 0.0725(3) 0.0251(6) Uani 1 1 d . . . . .
C11 C -0.0096(4) 0.3325(4) 0.0093(4) 0.0376(8) Uani 1 1 d . . . . .
H11A H -0.0685 0.2919 0.0488 0.045 Uiso 1 1 calc R U . . .
H11B H -0.0298 0.3701 -0.0874 0.045 Uiso 1 1 calc R U . . .
C12 C -0.0421(4) 0.4646(4) 0.0297(4) 0.0332(8) Uani 1 1 d . . . . .
H12A H -0.1388 0.5429 -0.0115 0.040 Uiso 1 1 calc R U . . .
H12B H -0.0262 0.4280 0.1264 0.040 Uiso 1 1 calc R U . . .
C14 C 0.3272(4) 0.0265(4) 0.2002(3) 0.0294(7) Uani 1 1 d . . . . .
H14 H 0.3994 -0.0527 0.2769 0.035 Uiso 1 1 calc R U . . .
C15 C 0.1959(4) 0.1130(4) 0.2001(4) 0.0332(8) Uani 1 1 d . . . . .
C16 C 0.1244(5) 0.1128(4) 0.3094(4) 0.0443(10) Uani 1 1 d . . . . .
H16A H 0.1339 0.1765 0.3385 0.053 Uiso 1 1 calc R U . . .
H16B H 0.0271 0.1585 0.2741 0.053 Uiso 1 1 calc R U . . .
C17 C 0.1776(5) -0.0416(5) 0.4262(4) 0.0469(10) Uani 1 1 d . . . . .
H17A H 0.1602 -0.1024 0.4001 0.070 Uiso 1 1 calc R U . . .
H17B H 0.1327 -0.0347 0.4971 0.070 Uiso 1 1 calc R U . . .
H17C H 0.2751 -0.0898 0.4586 0.070 Uiso 1 1 calc R U . . .
N23 N 0.5999(3) -0.0044(3) 0.1359(3) 0.0261(6) Uani 1 1 d . . . . .
C23 C 0.6474(4) -0.0188(4) 0.2290(3) 0.0308(7) Uani 1 1 d . . . . .
C231 C 0.7076(5) -0.0395(5) 0.3507(4) 0.0446(10) Uani 1 1 d . . . . .
H23A H 0.6487 0.0480 0.3603 0.067 Uiso 1 1 calc R U . . .
H23B H 0.7961 -0.0488 0.3459 0.067 Uiso 1 1 calc R U . . .
H23C H 0.7183 -0.1318 0.4276 0.067 Uiso 1 1 calc R U . . .
Cl1 Cl 0.36171(9) 0.33523(9) 0.30131(8) 0.0313(2) Uani 1 1 d . . . . .
O1 O 0.4663(3) 0.2270(4) 0.4218(3) 0.0545(8) Uani 1 1 d . . . . .
O2 O 0.3989(4) 0.2908(4) 0.2046(3) 0.0588(9) Uani 1 1 d . . . . .
O3 O 0.2413(4) 0.3390(5) 0.3275(4) 0.0803(12) Uani 1 1 d . . . . .
O4 O 0.3485(4) 0.4786(4) 0.2563(3) 0.0678(10) Uani 1 1 d . . . . .
C99 C 0.1355(7) 0.9255(7) -0.0504(8) 0.0785(19) Uani 1 1 d . . . . .
N99 N 0.0419(10) 1.0114(9) -0.1654(6) 0.123(3) Uani 1 1 d . . . . .
C98 C 0.2262(4) 0.8347(4) 0.0860(4) 0.0441(10) Uani 1 1 d . . . . .
H98A H 0.1728 0.8566 0.1476 0.066 Uiso 1 1 calc R U . . .
H98B H 0.2955 0.8616 0.0832 0.066 Uiso 1 1 calc R U . . .
H98C H 0.2696 0.7264 0.1166 0.066 Uiso 1 1 calc R U . . .
N88 N 0.9462(4) -0.5730(6) 0.3689(4) 0.0635(12) Uani 1 1 d . . . . .
C89 C 0.9623(5) -0.4728(7) 0.3419(5) 0.0574(12) Uani 1 1 d . . . . .
C88 C 0.9851(6) -0.3495(6) 0.3100(5) 0.0705(16) Uani 1 1 d . . . . .
H88A H 0.9689 -0.3240 0.3804 0.106 Uiso 1 1 calc R U . . .
H88B H 0.9234 -0.2607 0.2249 0.106 Uiso 1 1 calc R U . . .
H88C H 1.0786 -0.3807 0.3032 0.106 Uiso 1 1 calc R U . . .


_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 N23 1.949(3) . ?
Fe1 N23 1.949(3) 2_655 ?
Fe1 N3 2.008(2) . ?
Fe1 N3 2.008(2) 2_655 ?
Fe1 N13 2.027(3) 2_655 ?
Fe1 N13 2.027(3) . ?
N1 N2 1.339(3) . ?
N1 C5 1.350(4) . ?
N1 C1 1.472(4) . ?
N2 N3 1.322(4) . ?
N3 C4 1.361(4) . ?
C1 C2 1.527(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.516(6) 2_646 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C5 1.372(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.494(4) . ?
C6 C7 1.517(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N11 N12 1.341(4) . ?
N11 C15 1.350(5) . ?
N11 C11 1.470(5) . ?
N12 N13 1.316(4) . ?
N13 C14 1.350(4) . ?
C11 C12 1.527(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.513(7) 2_565 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.372(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.502(5) . ?
C16 C17 1.484(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N23 C23 1.134(4) . ?
C23 C231 1.459(5) . ?
C231 H23A 0.9800 . ?
C231 H23B 0.9800 . ?
C231 H23C 0.9800 . ?
Cl1 O3 1.402(4) . ?
Cl1 O4 1.422(3) . ?
Cl1 O2 1.424(3) . ?
Cl1 O1 1.432(3) . ?
C99 N99 1.339(10) . ?
C99 C98 1.497(9) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
N88 C89 1.158(7) . ?
C89 C88 1.451(8) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?

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
N23 Fe1 N23 180.0 . 2_655 ?
N23 Fe1 N3 89.06(10) . . ?
N23 Fe1 N3 90.94(10) 2_655 . ?
N23 Fe1 N3 90.94(10) . 2_655 ?
N23 Fe1 N3 89.06(10) 2_655 2_655 ?
N3 Fe1 N3 180.0 . 2_655 ?
N23 Fe1 N13 92.41(11) . 2_655 ?
N23 Fe1 N13 87.59(11) 2_655 2_655 ?
N3 Fe1 N13 88.23(10) . 2_655 ?
N3 Fe1 N13 91.77(10) 2_655 2_655 ?
N23 Fe1 N13 87.59(11) . . ?
N23 Fe1 N13 92.41(11) 2_655 . ?
N3 Fe1 N13 91.77(10) . . ?
N3 Fe1 N13 88.23(10) 2_655 . ?
N13 Fe1 N13 180.0 2_655 . ?
N2 N1 C5 112.2(2) . . ?
N2 N1 C1 118.9(2) . . ?
C5 N1 C1 128.8(2) . . ?
N3 N2 N1 106.0(2) . . ?
N2 N3 C4 109.6(2) . . ?
N2 N3 Fe1 121.7(2) . . ?
C4 N3 Fe1 128.4(2) . . ?
N1 C1 C2 113.0(3) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 113.0(3) 2_646 . ?
C2 C2 H2A 109.0 2_646 . ?
C1 C2 H2A 109.0 . . ?
C2 C2 H2B 109.0 2_646 . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N3 C4 C5 108.1(3) . . ?
N3 C4 H4 126.0 . . ?
C5 C4 H4 126.0 . . ?
N1 C5 C4 104.2(3) . . ?
N1 C5 C6 123.6(3) . . ?
C4 C5 C6 132.2(3) . . ?
C5 C6 C7 113.1(3) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 N11 C15 111.6(3) . . ?
N12 N11 C11 119.8(3) . . ?
C15 N11 C11 128.5(3) . . ?
N13 N12 N11 106.2(3) . . ?
N12 N13 C14 109.8(3) . . ?
N12 N13 Fe1 120.9(2) . . ?
C14 N13 Fe1 129.3(2) . . ?
N11 C11 C12 112.6(3) . . ?
N11 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N11 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C12 C12 C11 112.7(4) 2_565 . ?
C12 C12 H12A 109.1 2_565 . ?
C11 C12 H12A 109.1 . . ?
C12 C12 H12B 109.1 2_565 . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N13 C14 C15 108.2(3) . . ?
N13 C14 H14 125.9 . . ?
C15 C14 H14 125.9 . . ?
N11 C15 C14 104.2(3) . . ?
N11 C15 C16 122.8(3) . . ?
C14 C15 C16 133.0(3) . . ?
C17 C16 C15 112.8(3) . . ?
C17 C16 H16A 109.0 . . ?
C15 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
C15 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 168.2(3) . . ?
N23 C23 C231 178.7(4) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O3 Cl1 O4 111.1(2) . . ?
O3 Cl1 O2 109.8(3) . . ?
O4 Cl1 O2 110.2(2) . . ?
O3 Cl1 O1 109.0(2) . . ?
O4 Cl1 O1 107.7(2) . . ?
O2 Cl1 O1 109.0(2) . . ?
N99 C99 C98 173.0(6) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N88 C89 C88 178.8(6) . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.5(3) . . . . ?
C1 N1 N2 N3 178.3(2) . . . . ?
N1 N2 N3 C4 -0.2(3) . . . . ?
N1 N2 N3 Fe1 -174.49(18) . . . . ?
N2 N1 C1 C2 104.7(3) . . . . ?
C5 N1 C1 C2 -77.9(4) . . . . ?
N1 C1 C2 C2 -62.0(4) . . . 2_646 ?
N2 N3 C4 C5 -0.2(3) . . . . ?
Fe1 N3 C4 C5 173.6(2) . . . . ?
N2 N1 C5 C4 -0.7(3) . . . . ?
C1 N1 C5 C4 -178.2(3) . . . . ?
N2 N1 C5 C6 175.7(3) . . . . ?
C1 N1 C5 C6 -1.8(5) . . . . ?
N3 C4 C5 N1 0.5(3) . . . . ?
N3 C4 C5 C6 -175.4(3) . . . . ?
N1 C5 C6 C7 168.3(3) . . . . ?
C4 C5 C6 C7 -16.4(5) . . . . ?
C15 N11 N12 N13 0.2(3) . . . . ?
C11 N11 N12 N13 178.1(3) . . . . ?
N11 N12 N13 C14 -0.4(3) . . . . ?
N11 N12 N13 Fe1 -178.26(18) . . . . ?
N12 N11 C11 C12 -108.3(4) . . . . ?
C15 N11 C11 C12 69.3(4) . . . . ?
N11 C11 C12 C12 59.7(5) . . . 2_565 ?
N12 N13 C14 C15 0.5(4) . . . . ?
Fe1 N13 C14 C15 178.1(2) . . . . ?
N12 N11 C15 C14 0.2(4) . . . . ?
C11 N11 C15 C14 -177.6(3) . . . . ?
N12 N11 C15 C16 -179.1(3) . . . . ?
C11 N11 C15 C16 3.1(5) . . . . ?
N13 C14 C15 N11 -0.4(4) . . . . ?
N13 C14 C15 C16 178.8(4) . . . . ?
N11 C15 C16 C17 144.3(4) . . . . ?
C14 C15 C16 C17 -34.7(6) . . . . ?

_refine_diff_density_max         2.032
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_rb17_68_4a_145k
_database_code_depnum_ccdc_archive 'CCDC 1573883'
_audit_update_record             
;
2017-09-11 deposited with the CCDC.
2018-03-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C28 H46 Fe N14, 2(Cl O4), 4(C2 H3 N)
;
_chemical_formula_sum            'C36 H58 Cl2 Fe N18 O8'
_chemical_formula_weight         997.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4824(4)
_cell_length_b                   11.6432(5)
_cell_length_c                   11.8553(4)
_cell_angle_alpha                63.433(4)
_cell_angle_beta                 90.777(3)
_cell_angle_gamma                63.339(4)
_cell_volume                     1220.53(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    145(1)
_cell_measurement_reflns_used    5394
_cell_measurement_theta_min      3.3790
_cell_measurement_theta_max      35.5930

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.484
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      145(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            10391
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.229
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4990
_reflns_number_gt                4270
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0496P)²+0.4706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4990
_refine_ls_number_parameters     300
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.045
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.01518(10) Uani 1 2 d S . P . .
N1 N 0.63170(14) -0.43003(16) 0.31860(13) 0.0176(3) Uani 1 1 d . . . . .
N2 N 0.58546(15) -0.28393(16) 0.26393(14) 0.0190(3) Uani 1 1 d . . . . .
N3 N 0.56200(15) -0.22983(16) 0.13600(13) 0.0186(3) Uani 1 1 d . . . . .
C1 C 0.67144(19) -0.5231(2) 0.46247(16) 0.0217(4) Uani 1 1 d . . . . .
H1A H 0.6831 -0.4678 0.5011 0.026 Uiso 1 1 calc R U . . .
H1B H 0.7598 -0.6147 0.4906 0.026 Uiso 1 1 calc R U . . .
C2 C 0.56830(18) -0.56670(19) 0.51500(17) 0.0210(4) Uani 1 1 d . . . . .
H2A H 0.5564 -0.6217 0.4762 0.025 Uiso 1 1 calc R U . . .
H2B H 0.6038 -0.6347 0.6110 0.025 Uiso 1 1 calc R U . . .
C4 C 0.59388(17) -0.34183(19) 0.11085(17) 0.0192(4) Uani 1 1 d . . . . .
H4 H 0.5859 -0.3317 0.0266 0.023 Uiso 1 1 calc R U . . .
C5 C 0.63953(17) -0.47204(19) 0.22785(17) 0.0189(4) Uani 1 1 d . . . . .
C6 C 0.6949(2) -0.6292(2) 0.26084(18) 0.0260(4) Uani 1 1 d . . . . .
H6A H 0.6533 -0.6748 0.3261 0.031 Uiso 1 1 calc R U . . .
H6B H 0.7936 -0.6860 0.3012 0.031 Uiso 1 1 calc R U . . .
C7 C 0.6692(2) -0.6418(2) 0.1420(2) 0.0328(5) Uani 1 1 d . . . . .
H7A H 0.5718 -0.5970 0.1083 0.049 Uiso 1 1 calc R U . . .
H7B H 0.7157 -0.7472 0.1671 0.049 Uiso 1 1 calc R U . . .
H7C H 0.7034 -0.5894 0.0740 0.049 Uiso 1 1 calc R U . . .
N11 N 0.12337(15) 0.21328(16) 0.07110(14) 0.0196(3) Uani 1 1 d . . . . .
N12 N 0.20755(15) 0.19199(16) -0.00409(14) 0.0209(3) Uani 1 1 d . . . . .
N13 N 0.32590(15) 0.07755(16) 0.07639(14) 0.0192(3) Uani 1 1 d . . . . .
C11 C -0.01726(18) 0.3378(2) 0.00982(19) 0.0246(4) Uani 1 1 d . . . . .
H11A H -0.0785 0.3010 0.0468 0.030 Uiso 1 1 calc R U . . .
H11B H -0.0391 0.3749 -0.0853 0.030 Uiso 1 1 calc R U . . .
C12 C -0.04259(18) 0.4659(2) 0.03048(18) 0.0237(4) Uani 1 1 d . . . . .
H12A H -0.0216 0.4291 0.1255 0.028 Uiso 1 1 calc R U . . .
H12B H -0.1395 0.5438 -0.0085 0.028 Uiso 1 1 calc R U . . .
C14 C 0.31618(18) 0.02717(19) 0.20149(17) 0.0213(4) Uani 1 1 d . . . . .
H14 H 0.3876 -0.0545 0.2775 0.026 Uiso 1 1 calc R U . . .
C15 C 0.18605(18) 0.11397(19) 0.19974(17) 0.0207(4) Uani 1 1 d . . . . .
C16 C 0.1163(2) 0.1112(2) 0.30622(19) 0.0280(4) Uani 1 1 d . . . . .
H16A H 0.0184 0.1557 0.2702 0.034 Uiso 1 1 calc R U . . .
H16B H 0.1268 0.1728 0.3374 0.034 Uiso 1 1 calc R U . . .
C17 C 0.1725(2) -0.0454(2) 0.42056(19) 0.0327(5) Uani 1 1 d . . . . .
H17A H 0.1557 -0.1047 0.3915 0.049 Uiso 1 1 calc R U . . .
H17B H 0.1280 -0.0418 0.4899 0.049 Uiso 1 1 calc R U . . .
H17C H 0.2701 -0.0914 0.4543 0.049 Uiso 1 1 calc R U . . .
N23 N 0.61347(16) -0.00273(17) 0.14947(15) 0.0232(3) Uani 1 1 d . . . . .
C23 C 0.6535(2) -0.0243(2) 0.24907(19) 0.0256(4) Uani 1 1 d . . . . .
C231 C 0.7044(3) -0.0539(3) 0.3781(2) 0.0476(6) Uani 1 1 d . . . . .
H23A H 0.6471 0.0330 0.3865 0.071 Uiso 1 1 calc R U . . .
H23B H 0.7973 -0.0734 0.3890 0.071 Uiso 1 1 calc R U . . .
H23C H 0.7029 -0.1411 0.4456 0.071 Uiso 1 1 calc R U . . .
Cl1 Cl 0.35886(5) 0.33895(5) 0.29019(4) 0.02804(13) Uani 1 1 d . . . . .
O1 O 0.46273(18) 0.2343(2) 0.41102(16) 0.0506(4) Uani 1 1 d . . . . .
O2 O 0.3989(2) 0.2966(2) 0.19541(18) 0.0623(5) Uani 1 1 d . . . . .
O3 O 0.23639(19) 0.3415(2) 0.3081(2) 0.0648(6) Uani 1 1 d . . . . .
O4 O 0.3415(2) 0.4825(2) 0.2469(2) 0.0731(6) Uani 1 1 d . . . . .
C99 C 0.1305(3) 0.9299(3) -0.0602(3) 0.0451(6) Uani 1 1 d . . . . .
N99 N 0.0541(3) 1.0053(3) -0.1634(3) 0.0628(6) Uani 1 1 d . U . . .
C98 C 0.2244(2) 0.8346(3) 0.0696(3) 0.0440(6) Uani 1 1 d . . . . .
H98A H 0.1759 0.8508 0.1332 0.066 Uiso 1 1 calc R U . . .
H98B H 0.2959 0.8589 0.0694 0.066 Uiso 1 1 calc R U . . .
H98C H 0.2648 0.7300 0.0935 0.066 Uiso 1 1 calc R U . . .
N88 N 0.9513(2) -0.5808(4) 0.3758(2) 0.0615(7) Uani 1 1 d . . . . .
C89 C 0.9648(2) -0.4798(4) 0.3451(2) 0.0503(7) Uani 1 1 d . . . . .
C88 C 0.9852(3) -0.3549(3) 0.3087(3) 0.0624(8) Uani 1 1 d . . . . .
H88A H 0.9755 -0.3300 0.3782 0.094 Uiso 1 1 calc R U . . .
H88B H 0.9178 -0.2685 0.2269 0.094 Uiso 1 1 calc R U . . .
H88C H 1.0762 -0.3818 0.2966 0.094 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.1603(14) 2_655 ?
Fe1 N3 2.1603(14) . ?
Fe1 N23 2.1652(16) 2_655 ?
Fe1 N23 2.1652(16) . ?
Fe1 N13 2.1892(14) 2_655 ?
Fe1 N13 2.1892(14) . ?
N1 N2 1.338(2) . ?
N1 C5 1.356(2) . ?
N1 C1 1.474(2) . ?
N2 N3 1.3235(19) . ?
N3 C4 1.359(2) . ?
C1 C2 1.525(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.518(3) 2_646 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C5 1.372(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.488(2) . ?
C6 C7 1.519(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N11 N12 1.340(2) . ?
N11 C15 1.352(2) . ?
N11 C11 1.470(2) . ?
N12 N13 1.317(2) . ?
N13 C14 1.357(2) . ?
C11 C12 1.519(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.521(4) 2_565 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.371(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.500(2) . ?
C16 C17 1.513(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N23 C23 1.134(2) . ?
C23 C231 1.457(3) . ?
C231 H23A 0.9800 . ?
C231 H23B 0.9800 . ?
C231 H23C 0.9800 . ?
Cl1 O3 1.4143(18) . ?
Cl1 O2 1.4224(18) . ?
Cl1 O4 1.4240(19) . ?
Cl1 O1 1.4310(17) . ?
C99 N99 1.165(4) . ?
C99 C98 1.454(4) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
N88 C89 1.150(4) . ?
C89 C88 1.450(5) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N3 180.00(8) 2_655 . ?
N3 Fe1 N23 88.70(6) 2_655 2_655 ?
N3 Fe1 N23 91.30(6) . 2_655 ?
N3 Fe1 N23 91.30(6) 2_655 . ?
N3 Fe1 N23 88.70(6) . . ?
N23 Fe1 N23 180.0 2_655 . ?
N3 Fe1 N13 91.07(5) 2_655 2_655 ?
N3 Fe1 N13 88.93(5) . 2_655 ?
N23 Fe1 N13 86.82(6) 2_655 2_655 ?
N23 Fe1 N13 93.18(6) . 2_655 ?
N3 Fe1 N13 88.93(5) 2_655 . ?
N3 Fe1 N13 91.07(5) . . ?
N23 Fe1 N13 93.18(6) 2_655 . ?
N23 Fe1 N13 86.82(6) . . ?
N13 Fe1 N13 180.0 2_655 . ?
N2 N1 C5 112.05(13) . . ?
N2 N1 C1 119.00(14) . . ?
C5 N1 C1 128.91(15) . . ?
N3 N2 N1 106.14(13) . . ?
N2 N3 C4 109.50(14) . . ?
N2 N3 Fe1 121.83(11) . . ?
C4 N3 Fe1 128.44(11) . . ?
N1 C1 C2 112.98(15) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C2 C2 C1 112.88(18) 2_646 . ?
C2 C2 H2A 109.0 2_646 . ?
C1 C2 H2A 109.0 . . ?
C2 C2 H2B 109.0 2_646 . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N3 C4 C5 108.38(15) . . ?
N3 C4 H4 125.8 . . ?
C5 C4 H4 125.8 . . ?
N1 C5 C4 103.93(15) . . ?
N1 C5 C6 123.77(15) . . ?
C4 C5 C6 132.20(16) . . ?
C5 C6 C7 112.69(16) . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 N11 C15 111.98(14) . . ?
N12 N11 C11 119.54(14) . . ?
C15 N11 C11 128.44(15) . . ?
N13 N12 N11 106.24(13) . . ?
N12 N13 C14 109.41(14) . . ?
N12 N13 Fe1 120.30(11) . . ?
C14 N13 Fe1 130.28(12) . . ?
N11 C11 C12 112.64(15) . . ?
N11 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
N11 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C12 112.22(19) . 2_565 ?
C11 C12 H12A 109.2 . . ?
C12 C12 H12A 109.2 2_565 . ?
C11 C12 H12B 109.2 . . ?
C12 C12 H12B 109.2 2_565 . ?
H12A C12 H12B 107.9 . . ?
N13 C14 C15 108.55(16) . . ?
N13 C14 H14 125.7 . . ?
C15 C14 H14 125.7 . . ?
N11 C15 C14 103.83(15) . . ?
N11 C15 C16 123.54(16) . . ?
C14 C15 C16 132.63(17) . . ?
C15 C16 C17 112.09(16) . . ?
C15 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 N23 Fe1 159.44(15) . . ?
N23 C23 C231 179.1(2) . . ?
C23 C231 H23A 109.5 . . ?
C23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
C23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
O3 Cl1 O2 109.36(13) . . ?
O3 Cl1 O4 110.17(14) . . ?
O2 Cl1 O4 109.52(13) . . ?
O3 Cl1 O1 110.14(12) . . ?
O2 Cl1 O1 109.21(12) . . ?
O4 Cl1 O1 108.42(13) . . ?
N99 C99 C98 179.1(3) . . ?
C99 C98 H98A 109.5 . . ?
C99 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C99 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
N88 C89 C88 178.6(3) . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 N3 0.42(19) . . . . ?
C1 N1 N2 N3 178.05(14) . . . . ?
N1 N2 N3 C4 -0.19(18) . . . . ?
N1 N2 N3 Fe1 -175.17(10) . . . . ?
N2 N1 C1 C2 104.84(18) . . . . ?
C5 N1 C1 C2 -78.0(2) . . . . ?
N1 C1 C2 C2 -62.8(2) . . . 2_646 ?
N2 N3 C4 C5 -0.1(2) . . . . ?
Fe1 N3 C4 C5 174.47(12) . . . . ?
N2 N1 C5 C4 -0.46(19) . . . . ?
C1 N1 C5 C4 -177.80(16) . . . . ?
N2 N1 C5 C6 176.35(16) . . . . ?
C1 N1 C5 C6 -1.0(3) . . . . ?
N3 C4 C5 N1 0.33(19) . . . . ?
N3 C4 C5 C6 -176.09(19) . . . . ?
N1 C5 C6 C7 169.84(17) . . . . ?
C4 C5 C6 C7 -14.3(3) . . . . ?
C15 N11 N12 N13 0.16(19) . . . . ?
C11 N11 N12 N13 177.94(15) . . . . ?
N11 N12 N13 C14 0.01(19) . . . . ?
N11 N12 N13 Fe1 -179.18(10) . . . . ?
N12 N11 C11 C12 -105.32(18) . . . . ?
C15 N11 C11 C12 72.0(2) . . . . ?
N11 C11 C12 C12 61.9(2) . . . 2_565 ?
N12 N13 C14 C15 -0.2(2) . . . . ?
Fe1 N13 C14 C15 178.91(12) . . . . ?
N12 N11 C15 C14 -0.3(2) . . . . ?
C11 N11 C15 C14 -177.79(17) . . . . ?
N12 N11 C15 C16 -179.76(16) . . . . ?
C11 N11 C15 C16 2.7(3) . . . . ?
N13 C14 C15 N11 0.3(2) . . . . ?
N13 C14 C15 C16 179.69(19) . . . . ?
N11 C15 C16 C17 146.73(18) . . . . ?
C14 C15 C16 C17 -32.6(3) . . . . ?

_refine_diff_density_max         0.576
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.053

