#------------------------------------------------------------------------------
#$Date: 2019-12-12 12:50:50 +0200 (Thu, 12 Dec 2019) $
#$Revision: 245020 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556532.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1556532
loop_
_publ_author_name
'Craze, A.R.'
'Sciortino, N.F.'
'Badbhade, M.M.'
'Kepert, C.J.'
'Marjo, C.E.'
'Li, F.'
_publ_section_title
;
 Investigation of the Spin Crossover Properties of Three Dinulear Fe(II)
 Triple Helicates by Variation of the Steric Nature of the Ligand Type
;
_journal_name_full               Inorganics
_journal_page_first              62
_journal_paper_doi               10.3390/inorganics5040062
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety
;
C63 H54 Fe2 N18, 2(B0.4 F0.8), 2(B F4), 
2(B0.6 F3.2), 2(C0.5 H0.75 N0.5), 0.5(C2 H3 N)
;
_chemical_formula_sum            'C65 H57 B4 F16 Fe2 N19.5'
_chemical_formula_weight         1570.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 107.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.131(4)
_cell_length_b                   17.391(4)
_cell_length_c                   21.069(4)
_cell_measurement_reflns_used    2494
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.26
_cell_volume                     7404(3)
_computing_cell_refinement       'ShelXL least squares'
_computing_data_collection       XDS
_computing_data_reduction        xprep
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50460
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.545
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       needle
_exptl_crystal_F_000             3198
_exptl_crystal_recrystallization_method
'diethyl ether vapour diffusion into acetonitrile'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         6995
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.416
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.1035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1280P)²+69.2223P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2930
_refine_ls_wR_factor_ref         0.3220
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4686
_reflns_number_total             6995
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            FL206_a.cif
_cod_data_source_block           fl206_a
_cod_original_formula_sum        'C65 H57 B4 F16 Fe2 N19.50'
_cod_database_code               1556532
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.990
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{B01C, B01B}
3. Restrained distances
 B01B-B01C
 1.42 with sigma of 0.02
 F00X-B01B = F00Y-B01C = F3-B01B = F009-B01C = F10-B01B = F00T-B01C = F00H-
 B01C = F1-B01B
 1.39 with sigma of 0.02
 C1-C2 \\sim C11A-C2
 with sigma of 0.02
4. Rigid bond restraints
 C3B', C4C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(B01C) = Uanis(B01B)
6. Rigid body (RIGU) restrains
 N1B, N2B, N1B', N2B', C1B, C2B, C3B, C1B', C2B', C3B'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F009, F00H, F00T, F00Y
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C5, C6, C7, C8, C11A, C12A, C13A, C14A, C15A, C16A, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C5A, C6A, C7A, C8A, C9A, C10A, C5A', C6A', C7A', C8A', C9A'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4B, C4C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: N1B(0.5) N2B(0.5) H2B(0.5) N1B'(0.5) N2B'(0.5) H2B'(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) C3(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C12A(0.5) C7(0.5)
 H7(0.5) C8(0.5) H8(0.5) C7A(0.5) H7A(0.5) C8A(0.5) C9A(0.5) H9A(0.5) C9(0.5)
 H9(0.5) C5A(0.5) C6A(0.5) H6A(0.5) C11A(0.5) H11A(0.5) H11B(0.5) C15A(0.5)
 C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C2(0.5) C13A(0.5) H13A(0.5) C14A(0.5)
 H14A(0.5) C7A'(0.5) H7A'(0.5) C8A'(0.5) C9A'(0.5) H9A'(0.5) C10A(0.5)
 H10A(0.5) C5A'(0.5) C6A'(0.5) H6A'(0.5) C1B(0.5) H1BA(0.5) C2B(0.5) H2BA(0.5)
 C3B(0.5) C4B(0.5) H4B(0.5) H11C(0.5) H11D(0.5) C1B'(0.5) H1B'(0.5) C2B'(0.5)
 H2BB(0.5) C3B'(0.5) C4C(0.5) H4C(0.5) F1(0.2) F3(0.2) F10(0.2) F00X(0.2)
 B01B(0.4) F009(0.8) F00H(0.8) F00T(0.8) F00Y(0.8) B01C(0.6) N2(0.5) C1AA(0.25)
 C2AA(0.25) H2AB(0.25) H2AC(0.25) H2AD(0.25) N01L(0.25) C4(0.25) H4D(0.25)
 H4E(0.25) H4F(0.25) C0AA(0.25)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11A(H11A,H11B), C11B(H11C,H11D)
8.b Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N5A(H5A), N2B(H2B), N2B'(H2B'), C5(H5), C6(H6), C7(H7), C8(H8),
 C1A(H1AA), C2A(H2AA), C4A(H4A), C7A(H7A), C9A(H9A), C9(H9), C6A(H6A),
 C16A(H16A), C17A(H17A), C13A(H13A), C14A(H14A), C18A(H18A), C20A(H20A),
 C21A(H21A), C7A'(H7A'), C9A'(H9A'), C10A(H10A), C6A'(H6A'), C1B(H1BA),
 C2B(H2BA), C4B(H4B), C6B(H6B), C7B(H7B), C9B(H9B), C10B(H10B), C1B'(H1B'),
 C2B'(H2BB), C4C(H4C)
8.c Fitted hexagon refined as free rotating group:
 C3(C5,C6,C12A,C7,C8), C7A(C8A,C9A,C9,C5A,C6A), C15A(C16A,C17A,C2,C13A,C14A),
 C7A'(C8A',C9A',C10A,C5A',C6A')
8.d Idealised Me refined as rotating group:
 C2AA(H2AB,H2AC,H2AD), C4(H4D,H4E,H4F)
;
_olex2_exptl_crystal_mounting_method 'mounted in parafin oil'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe 0.43984(5) 0.27763(6) 0.46040(5) 0.0507(3) Uani 1 1 d . . . . .
N1A N 0.3882(4) 0.3668(4) 0.4013(3) 0.0650(18) Uani 1 1 d . . . . .
N2A N 0.3417(4) 0.4647(6) 0.3368(4) 0.088(3) Uani 1 1 d . . . . .
H2A H 0.3330 0.4970 0.3044 0.105 Uiso 1 1 calc R . . . .
N3A N 0.3649(3) 0.3069(4) 0.5090(3) 0.0516(14) Uani 1 1 d . . . . .
N4A N 0.5214(3) 0.1771(4) 0.9804(3) 0.0496(14) Uani 1 1 d . . . . .
N5A N 0.6784(4) 0.1039(6) 1.1601(4) 0.083(2) Uani 1 1 d . . . . .
H5A H 0.7090 0.0843 1.1924 0.099 Uiso 1 1 calc R . . . .
N6A N 0.6155(3) 0.1892(4) 1.0965(3) 0.0575(16) Uani 1 1 d . . . . .
N1B N 0.5256(11) 0.2769(13) 0.4175(11) 0.048(4) Uani 0.5 1 d . U . A 1
N2B N 0.6108(10) 0.2669(11) 0.3780(11) 0.060(4) Uani 0.5 1 d . U . A 1
H2B H 0.6338 0.2535 0.3522 0.072 Uiso 0.5 1 calc R . . A 1
N3B N 0.5135(3) 0.3527(4) 0.5208(3) 0.0511(14) Uani 1 1 d . . . . .
N1B' N 0.5057(12) 0.2611(16) 0.4139(13) 0.067(6) Uani 0.5 1 d . U . A 2
N2B' N 0.5802(11) 0.2410(11) 0.3593(8) 0.064(4) Uani 0.5 1 d . U . A 2
H2B' H 0.5975 0.2211 0.3309 0.077 Uiso 0.5 1 calc R . . A 2
C1 C 0.3183(11) 0.1359(16) 0.7290(8) 0.076(7) Uani 0.5 1 d D U . B 2
H1A H 0.3159 0.0817 0.7177 0.091 Uiso 0.5 1 calc R . . B 2
H1B H 0.2756 0.1512 0.7335 0.091 Uiso 0.5 1 calc R . . B 2
C3 C 0.4705(7) 0.1811(10) 0.9185(4) 0.046(5) Uani 0.5 1 d . U . C 1
C5 C 0.4848(4) 0.1867(7) 0.8583(4) 0.048(3) Uani 0.5 1 d G U . C 1
H5 H 0.5285 0.1904 0.8576 0.058 Uiso 0.5 1 calc R . . C 1
C6 C 0.4337(5) 0.1867(8) 0.7991(4) 0.055(4) Uani 0.5 1 d G U . C 1
H6 H 0.4433 0.1905 0.7589 0.065 Uiso 0.5 1 calc R . . C 1
C12A C 0.3684(4) 0.1812(8) 0.8001(5) 0.047(4) Uani 0.5 1 d G U . C 1
C7 C 0.3541(5) 0.1756(11) 0.8603(7) 0.048(5) Uani 0.5 1 d G U . C 1
H7 H 0.3104 0.1718 0.8610 0.058 Uiso 0.5 1 calc R . . C 1
C8 C 0.4052(8) 0.1756(12) 0.9195(5) 0.050(5) Uani 0.5 1 d G U . C 1
H8 H 0.3956 0.1718 0.9598 0.059 Uiso 0.5 1 calc R . . C 1
C1A C 0.3848(6) 0.4061(7) 0.3468(4) 0.085(3) Uani 1 1 d . . . . .
H1AA H 0.4097 0.3944 0.3183 0.102 Uiso 1 1 calc R . . . .
C2A C 0.3144(5) 0.4628(6) 0.3883(5) 0.080(3) Uani 1 1 d . . . . .
H2AA H 0.2828 0.4964 0.3953 0.097 Uiso 1 1 calc R . . . .
C3A C 0.3427(4) 0.4021(5) 0.4271(4) 0.063(2) Uani 1 1 d . . . . .
C4A C 0.3314(4) 0.3674(5) 0.4850(4) 0.062(2) Uani 1 1 d . . . . .
H4A H 0.3009 0.3881 0.5044 0.074 Uiso 1 1 calc R . . . .
C7A C 0.3339(9) 0.2925(8) 0.6713(8) 0.050(4) Uani 0.5 1 d . U . C 1
H7A H 0.3306 0.3236 0.7061 0.060 Uiso 0.5 1 calc R . . C 1
C8A C 0.3240(10) 0.2137(8) 0.6735(7) 0.045(4) Uani 0.5 1 d G U . C 1
C9A C 0.3288(12) 0.1672(10) 0.6215(9) 0.048(4) Uani 0.5 1 d G U . C 1
H9A H 0.3222 0.1144 0.6230 0.058 Uiso 0.5 1 calc R . . C 1
C9 C 0.3435(16) 0.1996(14) 0.5671(10) 0.050(6) Uani 0.5 1 d G U . C 1
H9 H 0.3468 0.1685 0.5323 0.060 Uiso 0.5 1 calc R . . C 1
C5A C 0.3534(15) 0.2785(14) 0.5649(9) 0.047(5) Uani 0.5 1 d G U . C 1
C6A C 0.3486(10) 0.3249(10) 0.6170(9) 0.047(4) Uani 0.5 1 d G U . C 1
H6A H 0.3551 0.3777 0.6154 0.057 Uiso 0.5 1 calc R . . C 1
C11A C 0.3112(8) 0.1756(12) 0.7365(7) 0.052(5) Uani 0.5 1 d D U . C 1
H11A H 0.2727 0.1997 0.7441 0.063 Uiso 0.5 1 calc R . . C 1
H11B H 0.3008 0.1217 0.7270 0.063 Uiso 0.5 1 calc R . . C 1
C15A C 0.4700(7) 0.1641(11) 0.9178(4) 0.045(5) Uani 0.5 1 d . U . B 2
C16A C 0.4854(5) 0.1305(9) 0.8643(5) 0.069(5) Uani 0.5 1 d G U . B 2
H16A H 0.5282 0.1132 0.8690 0.083 Uiso 0.5 1 calc R . . B 2
C17A C 0.4368(6) 0.1227(9) 0.8038(5) 0.073(4) Uani 0.5 1 d G U . B 2
H17A H 0.4471 0.1002 0.7680 0.088 Uiso 0.5 1 calc R . . B 2
C2 C 0.3729(5) 0.1485(9) 0.7967(5) 0.062(5) Uani 0.5 1 d DG U . B 2
C13A C 0.3575(6) 0.1821(11) 0.8502(7) 0.048(4) Uani 0.5 1 d G U . B 2
H13A H 0.3147 0.1994 0.8455 0.058 Uiso 0.5 1 calc R . . B 2
C14A C 0.4060(8) 0.1899(12) 0.9108(6) 0.047(4) Uani 0.5 1 d G U . B 2
H14A H 0.3957 0.2124 0.9466 0.056 Uiso 0.5 1 calc R . . B 2
C18A C 0.5456(4) 0.1135(5) 1.0076(3) 0.0567(19) Uani 1 1 d . . . . .
H18A H 0.5304 0.0664 0.9881 0.068 Uiso 1 1 calc R . . . .
C19A C 0.5976(4) 0.1179(5) 1.0699(3) 0.0571(19) Uani 1 1 d . . . . .
C20A C 0.6377(5) 0.0637(6) 1.1100(4) 0.079(3) Uani 1 1 d . . . . .
H20A H 0.6368 0.0107 1.1038 0.095 Uiso 1 1 calc R . . . .
C21A C 0.6644(4) 0.1777(6) 1.1520(4) 0.070(2) Uani 1 1 d . . . . .
H21A H 0.6856 0.2163 1.1809 0.084 Uiso 1 1 calc R . . . .
C7A' C 0.3437(11) 0.2607(9) 0.6793(8) 0.063(5) Uani 0.5 1 d . U . B 2
H7A' H 0.3446 0.2860 0.7184 0.075 Uiso 0.5 1 calc R . . B 2
C8A' C 0.3327(10) 0.1818(9) 0.6738(9) 0.054(5) Uani 0.5 1 d G U . B 2
C9A' C 0.3314(12) 0.1440(11) 0.6153(11) 0.055(5) Uani 0.5 1 d G U . B 2
H9A' H 0.3240 0.0912 0.6116 0.066 Uiso 0.5 1 calc R . . B 2
C10A C 0.3411(17) 0.1850(16) 0.5623(10) 0.059(6) Uani 0.5 1 d G U . B 2
H10A H 0.3403 0.1597 0.5232 0.071 Uiso 0.5 1 calc R . . B 2
C5A' C 0.3522(17) 0.2639(16) 0.5678(9) 0.055(6) Uani 0.5 1 d G U . B 2
C6A' C 0.3535(13) 0.3017(10) 0.6263(10) 0.067(6) Uani 0.5 1 d G U . B 2
H6A' H 0.3608 0.3544 0.6300 0.080 Uiso 0.5 1 calc R . . B 2
C1B C 0.5476(13) 0.2467(13) 0.3712(11) 0.061(4) Uani 0.5 1 d . U . A 1
H1BA H 0.5227 0.2151 0.3375 0.073 Uiso 0.5 1 calc R . . A 1
C2B C 0.6314(11) 0.3109(11) 0.4312(11) 0.057(4) Uani 0.5 1 d . U . A 1
H2BA H 0.6731 0.3328 0.4477 0.068 Uiso 0.5 1 calc R . . A 1
C3B C 0.5793(11) 0.3182(13) 0.4578(11) 0.047(4) Uani 0.5 1 d . U . A 1
C4B C 0.568(2) 0.363(2) 0.5132(18) 0.066(9) Uani 0.5 1 d . U . A 1
H4B H 0.5991 0.3964 0.5396 0.079 Uiso 0.5 1 calc R . . A 1
C5B C 0.5108(3) 0.3948(4) 0.5789(4) 0.0498(16) Uani 1 1 d . . . . .
C6B C 0.4680(4) 0.4571(4) 0.5716(4) 0.0529(17) Uani 1 1 d . . . . .
H6B H 0.4419 0.4718 0.5296 0.063 Uiso 1 1 calc R . . . .
C7B C 0.4646(4) 0.4971(4) 0.6279(4) 0.0514(17) Uani 1 1 d . . . . .
H7B H 0.4360 0.5388 0.6229 0.062 Uiso 1 1 calc R . . . .
C8B C 0.5027(4) 0.4764(4) 0.6908(4) 0.0542(17) Uani 1 1 d . . . . .
C9B C 0.5440(5) 0.4148(5) 0.6959(4) 0.070(2) Uani 1 1 d . . . . .
H9B H 0.5698 0.3996 0.7378 0.084 Uiso 1 1 calc R . . . .
C10B C 0.5487(4) 0.3742(5) 0.6412(4) 0.068(2) Uani 1 1 d . . . . .
H10B H 0.5777 0.3328 0.6467 0.081 Uiso 1 1 calc R . . . .
C11B C 0.5000 0.5234(6) 0.7500 0.064(3) Uani 1 2 d S T P . .
H11C H 0.5387 0.5563 0.7630 0.077 Uiso 0.5 1 calc R . . . .
H11D H 0.4613 0.5563 0.7370 0.077 Uiso 0.5 1 calc R . . . .
C1B' C 0.5183(12) 0.2265(14) 0.3629(11) 0.069(5) Uani 0.5 1 d . U . A 2
H1B' H 0.4879 0.1957 0.3327 0.082 Uiso 0.5 1 calc R . . A 2
C2B' C 0.6089(12) 0.2893(14) 0.4051(11) 0.062(5) Uani 0.5 1 d . U . A 2
H2BB H 0.6508 0.3107 0.4129 0.074 Uiso 0.5 1 calc R . . A 2
C3B' C 0.5641(17) 0.3023(16) 0.4398(12) 0.060(6) Uani 0.5 1 d . U . A 2
C4C C 0.5689(14) 0.3473(19) 0.5003(17) 0.043(5) Uani 0.5 1 d . U . A 2
H4C H 0.6083 0.3710 0.5237 0.052 Uiso 0.5 1 calc R . . A 2
F1 F 0.322(5) 0.612(2) 0.670(4) 0.19(4) Uiso 0.2 1 d D . . D 2
F3 F 0.2589(12) 0.5591(15) 0.6015(10) 0.077(7) Uiso 0.2 1 d D . . D 2
F10 F 0.328(2) 0.4653(15) 0.658(2) 0.125(12) Uiso 0.2 1 d D . . D 2
F00X F 0.2514(12) 0.5252(14) 0.7000(12) 0.051(6) Uiso 0.2 1 d D . . D 2
B01B B 0.2995(5) 0.5359(6) 0.6637(5) 0.082(3) Uani 0.4 1 d D . . D 2
F002 F 0.7305(3) 0.3772(4) 0.7071(2) 0.0837(16) Uani 1 1 d . . . . .
F003 F 0.8042(3) 0.2906(3) 0.6903(3) 0.0932(18) Uani 1 1 d . . . . .
F008 F 0.7246(3) 0.3416(4) 0.6032(3) 0.104(2) Uani 1 1 d . . . . .
F00A F 0.8087(3) 0.4157(4) 0.6617(4) 0.108(2) Uani 1 1 d . . . . .
B01A B 0.7666(5) 0.3561(7) 0.6663(5) 0.069(3) Uani 1 1 d . . . . .
F009 F 0.3272(4) 0.4763(4) 0.7040(3) 0.0810(19) Uani 0.8 1 d D U . E 1
F00H F 0.3414(7) 0.5982(7) 0.6871(5) 0.117(5) Uani 0.8 1 d D U . E 1
F00T F 0.3011(5) 0.5125(6) 0.5993(3) 0.112(3) Uani 0.8 1 d D U . E 1
F00Y F 0.2390(4) 0.5519(6) 0.6675(7) 0.138(5) Uani 0.8 1 d D U . E 1
B01C B 0.2995(5) 0.5359(6) 0.6637(5) 0.082(3) Uani 0.6 1 d D . . E 1
N2 N 0.4363(9) 0.0431(10) 1.0769(9) 0.088(5) Uiso 0.5 1 d . . . . .
C1AA C 0.3917(11) 0.0562(12) 1.0514(11) 0.029(4) Uiso 0.25 1 d . . . . .
C2AA C 0.3289(12) 0.0724(14) 1.0206(13) 0.040(5) Uiso 0.25 1 d . . . . .
H2AB H 0.3230 0.0773 0.9738 0.060 Uiso 0.25 1 calc GR . . . .
H2AC H 0.3170 0.1198 1.0374 0.060 Uiso 0.25 1 calc GR . . . .
H2AD H 0.3013 0.0317 1.0281 0.060 Uiso 0.25 1 calc GR . . . .
N01L N 0.5516(9) -0.1381(10) 0.7422(10) 0.033(4) Uiso 0.25 1 d . . . F 1
C4 C 0.5777(17) 0.0031(17) 0.7357(17) 0.061(7) Uiso 0.25 1 d . . . F 1
H4D H 0.5467 0.0268 0.6981 0.092 Uiso 0.25 1 calc GR . . F 1
H4E H 0.6215 0.0072 0.7312 0.092 Uiso 0.25 1 calc GR . . F 1
H4F H 0.5761 0.0286 0.7756 0.092 Uiso 0.25 1 calc GR . . F 1
C0AA C 0.5601(12) -0.0806(13) 0.7390(12) 0.035(5) Uiso 0.25 1 d . . . F 1
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1A Fe01 N3A 77.4(2) . .
N1A Fe01 N4A 171.2(2) . 2_656
N1A Fe01 N1B 96.1(6) . .
N1A Fe01 N3B 93.7(3) . .
N3A Fe01 N1B 166.0(6) . .
N4A Fe01 N3A 97.0(2) 2_656 .
N4A Fe01 N1B 90.8(6) 2_656 .
N6A Fe01 N1A 95.6(3) 2_656 .
N6A Fe01 N3A 94.6(2) 2_656 .
N6A Fe01 N4A 77.8(2) 2_656 2_656
N6A Fe01 N1B 98.4(6) 2_656 .
N6A Fe01 N3B 168.1(2) 2_656 .
N3B Fe01 N3A 94.6(2) . .
N3B Fe01 N4A 93.6(2) . 2_656
N3B Fe01 N1B 73.2(6) . .
N1B' Fe01 N1A 97.8(9) . .
N1B' Fe01 N3A 174.7(9) . .
N1B' Fe01 N4A 88.0(9) . 2_656
N1B' Fe01 N6A 88.0(7) . 2_656
N1B' Fe01 N3B 83.5(7) . .
C1A N1A Fe01 142.2(8) . .
C1A N1A C3A 104.2(8) . .
C3A N1A Fe01 113.5(5) . .
C1A N2A H2A 126.9 . .
C1A N2A C2A 106.3(8) . .
C2A N2A H2A 126.9 . .
C4A N3A Fe01 113.5(5) . .
C4A N3A C5A 114.8(13) . .
C4A N3A C5A' 120.6(13) . .
C5A N3A Fe01 131.1(13) . .
C5A' N3A Fe01 125.9(13) . .
C3 N4A Fe01 123.0(8) . 2_656
C15A N4A Fe01 134.6(8) . 2_656
C18A N4A Fe01 113.9(5) . 2_656
C18A N4A C3 123.0(9) . .
C18A N4A C15A 111.3(9) . .
C20A N5A H5A 125.2 . .
C21A N5A H5A 125.2 . .
C21A N5A C20A 109.7(8) . .
C19A N6A Fe01 113.1(5) . 2_656
C21A N6A Fe01 141.0(7) . 2_656
C21A N6A C19A 106.0(7) . .
C1B N1B Fe01 143.8(19) . .
C1B N1B C3B 104.8(18) . .
C3B N1B Fe01 111.0(13) . .
C1B N2B H2B 125.9 . .
C2B N2B H2B 125.9 . .
C2B N2B C1B 108.1(17) . .
C4B N3B Fe01 124.2(15) . .
C4B N3B C5B 108.0(15) . .
C5B N3B Fe01 127.7(4) . .
C4C N3B Fe01 108.2(12) . .
C4C N3B C5B 123.6(13) . .
C1B' N1B' Fe01 145.1(19) . .
C1B' N1B' C3B' 100.7(19) . .
C3B' N1B' Fe01 114.2(17) . .
C1B' N2B' H2B' 125.4 . .
C2B' N2B' H2B' 125.4 . .
C2B' N2B' C1B' 109.2(19) . .
H1A C1 H1B 108.0 . .
C2 C1 H1A 109.3 . .
C2 C1 H1B 109.3 . .
C8A' C1 H1A 109.3 . .
C8A' C1 H1B 109.3 . .
C8A' C1 C2 111.4(17) . .
C5 C3 N4A 122.0(9) . .
C5 C3 C8 120.0 . .
C8 C3 N4A 117.9(9) . .
C3 C5 H5 120.0 . .
C6 C5 C3 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 H6 120.0 . .
C5 C6 C12A 120.0 . .
C12A C6 H6 120.0 . .
C6 C12A C11A 121.8(10) . .
C7 C12A C6 120.0 . .
C7 C12A C11A 118.1(10) . .
C12A C7 H7 120.0 . .
C12A C7 C8 120.0 . .
C8 C7 H7 120.0 . .
C3 C8 H8 120.0 . .
C7 C8 C3 120.0 . .
C7 C8 H8 120.0 . .
N1A C1A N2A 113.2(9) . .
N1A C1A H1AA 123.4 . .
N2A C1A H1AA 123.4 . .
N2A C2A H2AA 126.8 . .
C3A C2A N2A 106.4(9) . .
C3A C2A H2AA 126.8 . .
N1A C3A C4A 117.0(7) . .
C2A C3A N1A 110.0(8) . .
C2A C3A C4A 132.9(9) . .
N3A C4A C3A 117.8(7) . .
N3A C4A H4A 121.1 . .
C3A C4A H4A 121.1 . .
C8A C7A H7A 120.0 . .
C8A C7A C6A 120.0 . .
C6A C7A H7A 120.0 . .
C7A C8A C11A 120.5(11) . .
C9A C8A C7A 120.0 . .
C9A C8A C11A 119.4(11) . .
C8A C9A H9A 120.0 . .
C8A C9A C9 120.0 . .
C9 C9A H9A 120.0 . .
C9A C9 H9 120.0 . .
C5A C9 C9A 120.0 . .
C5A C9 H9 120.0 . .
N3A C5A C9 117.0(15) . .
N3A C5A C6A 122.9(15) . .
C6A C5A C9 120.0 . .
C7A C6A H6A 120.0 . .
C5A C6A C7A 120.0 . .
C5A C6A H6A 120.0 . .
C12A C11A C8A 115.3(14) . .
C12A C11A H11A 108.5 . .
C12A C11A H11B 108.5 . .
C8A C11A H11A 108.5 . .
C8A C11A H11B 108.5 . .
H11A C11A H11B 107.5 . .
C16A C15A N4A 120.6(9) . .
C16A C15A C14A 120.0 . .
C14A C15A N4A 119.3(9) . .
C15A C16A H16A 120.0 . .
C15A C16A C17A 120.0 . .
C17A C16A H16A 120.0 . .
C16A C17A H17A 120.0 . .
C2 C17A C16A 120.0 . .
C2 C17A H17A 120.0 . .
C17A C2 C1 119.1(12) . .
C13A C2 C1 120.9(12) . .
C13A C2 C17A 120.0 . .
C2 C13A H13A 120.0 . .
C14A C13A C2 120.0 . .
C14A C13A H13A 120.0 . .
C15A C14A H14A 120.0 . .
C13A C14A C15A 120.0 . .
C13A C14A H14A 120.0 . .
N4A C18A H18A 121.4 . .
N4A C18A C19A 117.2(7) . .
C19A C18A H18A 121.4 . .
N6A C19A C18A 117.8(7) . .
N6A C19A C20A 108.8(8) . .
C20A C19A C18A 133.4(8) . .
N5A C20A C19A 105.3(9) . .
N5A C20A H20A 127.4 . .
C19A C20A H20A 127.4 . .
N5A C21A N6A 110.4(9) . .
N5A C21A H21A 124.8 . .
N6A C21A H21A 124.8 . .
C8A' C7A' H7A' 120.0 . .
C8A' C7A' C6A' 120.0 . .
C6A' C7A' H7A' 120.0 . .
C7A' C8A' C1 121.5(14) . .
C7A' C8A' C9A' 120.0 . .
C9A' C8A' C1 118.4(14) . .
C8A' C9A' H9A' 120.0 . .
C10A C9A' C8A' 120.0 . .
C10A C9A' H9A' 120.0 . .
C9A' C10A H10A 120.0 . .
C9A' C10A C5A' 120.0 . .
C5A' C10A H10A 120.0 . .
C10A C5A' N3A 118.5(15) . .
C6A' C5A' N3A 121.4(15) . .
C6A' C5A' C10A 120.0 . .
C7A' C6A' H6A' 120.0 . .
C5A' C6A' C7A' 120.0 . .
C5A' C6A' H6A' 120.0 . .
N1B C1B N2B 112(2) . .
N1B C1B H1BA 124.0 . .
N2B C1B H1BA 124.0 . .
N2B C2B H2BA 126.4 . .
N2B C2B C3B 107.1(18) . .
C3B C2B H2BA 126.4 . .
N1B C3B C4B 117(2) . .
C2B C3B N1B 108.0(17) . .
C2B C3B C4B 135(3) . .
N3B C4B C3B 114(3) . .
N3B C4B H4B 123.2 . .
C3B C4B H4B 123.2 . .
C6B C5B N3B 119.1(7) . .
C10B C5B N3B 121.6(7) . .
C10B C5B C6B 119.3(7) . .
C5B C6B H6B 120.4 . .
C5B C6B C7B 119.2(7) . .
C7B C6B H6B 120.4 . .
C6B C7B H7B 119.2 . .
C8B C7B C6B 121.7(7) . .
C8B C7B H7B 119.2 . .
C7B C8B C11B 120.0(7) . .
C9B C8B C7B 117.3(7) . .
C9B C8B C11B 122.6(7) . .
C8B C9B H9B 118.8 . .
C8B C9B C10B 122.4(8) . .
C10B C9B H9B 118.8 . .
C5B C10B C9B 120.1(7) . .
C5B C10B H10B 120.0 . .
C9B C10B H10B 120.0 . .
C8B C11B C8B 114.3(9) 2_656 .
C8B C11B H11C 108.7 . .
C8B C11B H11C 108.7 2_656 .
C8B C11B H11D 108.7 2_656 .
C8B C11B H11D 108.7 . .
H11C C11B H11D 107.6 . .
N1B' C1B' N2B' 113(2) . .
N1B' C1B' H1B' 123.6 . .
N2B' C1B' H1B' 123.6 . .
N2B' C2B' H2BB 127.5 . .
N2B' C2B' C3B' 105(2) . .
C3B' C2B' H2BB 127.5 . .
N1B' C3B' C4C 116(2) . .
C2B' C3B' N1B' 112(2) . .
C2B' C3B' C4C 132(3) . .
N3B C4C C3B' 117(2) . .
N3B C4C H4C 121.3 . .
C3B' C4C H4C 121.3 . .
F1 B01B F3 85(4) . .
F1 B01B F00X 110(4) . .
F3 B01B F00X 101.5(16) . .
F10 B01B F1 134(5) . .
F10 B01B F3 110(2) . .
F10 B01B F00X 109(2) . .
F002 B01A F003 111.0(7) . .
F002 B01A F008 109.5(8) . .
F002 B01A F00A 109.5(9) . .
F008 B01A F003 109.7(9) . .
F00A B01A F003 109.1(8) . .
F00A B01A F008 108.1(8) . .
F009 B01C F00H 105.0(10) . .
F009 B01C F00T 104.5(8) . .
F00H B01C F00T 111.6(9) . .
F00Y B01C F009 111.5(10) . .
F00Y B01C F00H 109.7(11) . .
F00Y B01C F00T 114.0(10) . .
N2 C1AA C2AA 175(3) . .
C1AA C2AA H2AB 109.5 . .
C1AA C2AA H2AC 109.5 . .
C1AA C2AA H2AD 109.5 . .
H2AB C2AA H2AC 109.5 . .
H2AB C2AA H2AD 109.5 . .
H2AC C2AA H2AD 109.5 . .
H4D C4 H4E 109.5 . .
H4D C4 H4F 109.5 . .
H4E C4 H4F 109.5 . .
C0AA C4 H4D 109.5 . .
C0AA C4 H4E 109.5 . .
C0AA C4 H4F 109.5 . .
N01L C0AA C4 176(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe01 N1A 2.086(7) .
Fe01 N3A 2.183(6) .
Fe01 N4A 2.164(6) 2_656
Fe01 N6A 2.085(7) 2_656
Fe01 N1B 2.250(17) .
Fe01 N3B 2.142(7) .
Fe01 N1B' 1.94(2) .
N1A C1A 1.320(11) .
N1A C3A 1.381(11) .
N2A H2A 0.8600 .
N2A C1A 1.341(14) .
N2A C2A 1.371(13) .
N3A C4A 1.286(10) .
N3A C5A 1.363(14) .
N3A C5A' 1.537(17) .
N4A Fe01 2.164(6) 2_656
N4A C3 1.429(10) .
N4A C15A 1.461(11) .
N4A C18A 1.282(10) .
N5A H5A 0.8600 .
N5A C20A 1.345(13) .
N5A C21A 1.317(12) .
N6A Fe01 2.085(7) 2_656
N6A C19A 1.367(10) .
N6A C21A 1.330(11) .
N1B C1B 1.31(2) .
N1B C3B 1.40(3) .
N2B H2B 0.8600 .
N2B C1B 1.35(3) .
N2B C2B 1.32(3) .
N3B C4B 1.22(4) .
N3B C5B 1.442(9) .
N3B C4C 1.36(2) .
N1B' C1B' 1.33(3) .
N1B' C3B' 1.39(3) .
N2B' H2B' 0.8600 .
N2B' C1B' 1.36(3) .
N2B' C2B' 1.29(3) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C1 C2 1.567(16) .
C1 C8A' 1.51(3) .
C3 C5 1.3900 .
C3 C8 1.3900 .
C5 H5 0.9300 .
C5 C6 1.3900 .
C6 H6 0.9300 .
C6 C12A 1.3900 .
C12A C7 1.3900 .
C12A C11A 1.523(15) .
C7 H7 0.9300 .
C7 C8 1.3900 .
C8 H8 0.9300 .
C1A H1AA 0.9300 .
C2A H2AA 0.9300 .
C2A C3A 1.362(12) .
C3A C4A 1.442(11) .
C4A H4A 0.9300 .
C7A H7A 0.9300 .
C7A C8A 1.3900 .
C7A C6A 1.3900 .
C8A C9A 1.3900 .
C8A C11A 1.57(2) .
C9A H9A 0.9300 .
C9A C9 1.3900 .
C9 H9 0.9300 .
C9 C5A 1.3900 .
C5A C6A 1.3900 .
C6A H6A 0.9300 .
C11A H11A 0.9700 .
C11A H11B 0.9700 .
C15A C16A 1.3900 .
C15A C14A 1.3900 .
C16A H16A 0.9300 .
C16A C17A 1.3900 .
C17A H17A 0.9300 .
C17A C2 1.3900 .
C2 C13A 1.3900 .
C13A H13A 0.9300 .
C13A C14A 1.3900 .
C14A H14A 0.9300 .
C18A H18A 0.9300 .
C18A C19A 1.447(11) .
C19A C20A 1.380(11) .
C20A H20A 0.9300 .
C21A H21A 0.9300 .
C7A' H7A' 0.9300 .
C7A' C8A' 1.3900 .
C7A' C6A' 1.3900 .
C8A' C9A' 1.3900 .
C9A' H9A' 0.9300 .
C9A' C10A 1.3900 .
C10A H10A 0.9300 .
C10A C5A' 1.3900 .
C5A' C6A' 1.3900 .
C6A' H6A' 0.9300 .
C1B H1BA 0.9300 .
C2B H2BA 0.9300 .
C2B C3B 1.38(2) .
C3B C4B 1.48(3) .
C4B H4B 0.9300 .
C5B C6B 1.390(10) .
C5B C10B 1.371(11) .
C6B H6B 0.9300 .
C6B C7B 1.395(10) .
C7B H7B 0.9300 .
C7B C8B 1.384(10) .
C8B C9B 1.366(11) .
C8B C11B 1.505(9) .
C9B H9B 0.9300 .
C9B C10B 1.379(12) .
C10B H10B 0.9300 .
C11B C8B 1.505(9) 2_656
C11B H11C 0.9700 .
C11B H11D 0.9700 .
C1B' H1B' 0.9300 .
C2B' H2BB 0.9300 .
C2B' C3B' 1.37(3) .
C3B' C4C 1.47(3) .
C4C H4C 0.9300 .
F1 B01B 1.39(2) .
F3 B01B 1.400(17) .
F10 B01B 1.389(19) .
F00X B01B 1.452(17) .
F002 B01A 1.356(10) .
F003 B01A 1.396(12) .
F008 B01A 1.389(12) .
F00A B01A 1.389(13) .
F009 B01C 1.359(11) .
F00H B01C 1.393(12) .
F00T B01C 1.426(11) .
F00Y B01C 1.333(12) .
N2 C1AA 0.97(2) .
C1AA C2AA 1.32(3) .
C2AA H2AB 0.9600 .
C2AA H2AC 0.9600 .
C2AA H2AD 0.9600 .
N01L C0AA 1.02(3) .
C4 H4D 0.9600 .
C4 H4E 0.9600 .
C4 H4F 0.9600 .
C4 C0AA 1.51(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5A H5A F00X 0.86 2.09 2.71(3) 128.8 8_556
N2B H2B F003 0.86 1.95 2.795(18) 167.7 7_656
C2AA H2AB F3 0.96 2.00 2.71(3) 128.4 4_546
