#------------------------------------------------------------------------------
#$Date: 2022-01-21 01:12:41 +0200 (Fri, 21 Jan 2022) $
#$Revision: 272167 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/60/1566083.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_1566083
loop_
_publ_author_name
'Shaw, Bikash Kumar'
'Bennett, Thomas Douglas'
'Castillo Blas, Celia'
'Thorne, Michael Francis'
'Gómez, María Laura Ríos'
'Forrest, Thomas'
'Keen, David A.'
'Diaz-Lopez, Maria'
'Chater, Philip A.'
'McHugh, Lauren Nicole'
_publ_section_title
;
 Principles of Melting in Hybrid Organic-Inorganic Perovskite and
 Polymorphic ABX3 Structures
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC07080K
_journal_year                    2022
_chemical_formula_moiety
'0.13(C48 Fe8 N72), 0.25(C32.02 H72.2 N2), 0.5(C16 H35.64 N)'
_chemical_formula_sum            'C22.01 H35.86 Fe N10'
_chemical_formula_weight         496.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-31 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7971(7)
_cell_length_b                   15.8093(9)
_cell_length_c                   21.4138(11)
_cell_measurement_reflns_used    8450
_cell_measurement_temperature    240
_cell_measurement_theta_max      64.632
_cell_measurement_theta_min      3.475
_cell_volume                     5347.9(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      240
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Vantec 500'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55212
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.338
_diffrn_reflns_theta_max         65.338
_diffrn_reflns_theta_min         2.063
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.747
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1429 before and 0.0966 after correction. The Ratio of minimum to maximum transmission is 0.6634. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'yellowish colourless'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       prism
_exptl_crystal_F_000             2111
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         9065
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.1063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1523P)²+21.3446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2999
_refine_ls_wR_factor_ref         0.3279
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6196
_reflns_number_total             9065
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc07080k2.cif
_cod_data_source_block           celiap21212
_cod_database_code               1566083
_shelx_shelxl_version_number     2014/7
_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   0.764
_shelx_estimated_absorpt_t_min   0.648
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(3)
 0.07(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Rigid bond restraints
 N11
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
4. Uiso/Uaniso restraints and constraints
Uanis(C62B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uiso(C51B) = Uiso(C51A)
Uanis(C54B) = Uanis(C54A)
Uanis(C50A) = Uanis(C62B)
Uanis(C72) = Uanis(C71B)
5. Others
 Sof(C55B)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(1)
 Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=FVAR(1)
 Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(2)
 Sof(H42A)=Sof(H42B)=Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(2)
 Sof(C51B)=Sof(H51A)=Sof(H51B)=1-FVAR(3)
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(H51E)=FVAR(3)
 Fixed Sof: C63B(0.33333) H63A(0.33333) H63B(0.33333) H63C(0.33333) C62A(0.67)
 H62A(0.67) H62B(0.67) H70C(0.7) H70D(0.7) H70A(0.33333) H70B(0.33333)
 H53C(0.5) H53D(0.5) H53A(0.5) H53B(0.5) C50A(0.33333) H50A(0.33333)
 H50B(0.33333) C50B(0.67) H50C(0.67) H50D(0.67) C54B(0.5) H54A(0.5) H54B(0.5)
 H72D(0.67) H72E(0.67) H72F(0.67) H72A(0.33333) H72B(0.33333) H72C(0.33333)
 C71B(0.67) H71A(0.67) H71B(0.67) C54A(0.5) H54C(0.5) H54D(0.5) C62B(0.33333)
 H62C(0.33333) H62D(0.33333) C71A(0.33333) H71C(0.33333) H71D(0.33333)
 C63A(0.67) H63D(0.67) H63E(0.67) H63F(0.67)
6.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C60(H60A,H60B), C66(H66A,H66B), C62A(H62A,H62B), C48(H48A,
 H48B), C70(H70C,H70D), C70(H70A,H70B), C40(H40A,H40B), C42(H42C,H42D),
 C42(H42A,H42B), C69(H69A,H69B), C65(H65A,H65B), C53(H53C,H53D), C53(H53A,H53B),
  C50A(H50A,H50B), C52(H52A,H52B), C45(H45A,H45B), C50B(H50C,H50D), C49(H49A,
 H49B), C44(H44A,H44B), C54B(H54A,H54B), C46(H46A,H46B), C73(H73A,H73B),
 C75(H75A,H75B), C71B(H71A,H71B), C74(H74A,H74B), C67(H67A,H67B), C51B(H51A,
 H51B), C54A(H54C,H54D), C41(H41A,H41B), C62B(H62C,H62D), C71A(H71C,H71D)
6.b Idealised Me refined as rotating group:
 C63B(H63A,H63B,H63C), C55B(H55A,H55B,H55C), C47(H47A,H47B,H47C), C72(H72D,
 H72E,H72F), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C43A(H43A,H43B,H43C),
 C68(H68A,H68B,H68C), C63A(H63D,H63E,H63F), C55A(H55D,H55E,H55F), C43B(H43D,
 H43E,H43F), C51A(H51C,H51D,H51E)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.68218(10) 0.0322(6) Uani 1 2 d S T P . .
Fe2 Fe 0.5000 1.0000 0.67252(10) 0.0350(6) Uani 1 2 d S T P . .
Fe3 Fe 1.0000 1.0000 0.82237(10) 0.0364(7) Uani 1 2 d S T P . .
Fe4 Fe 0.5000 0.5000 0.82290(10) 0.0353(6) Uani 1 2 d S T P . .
N12 N -0.0010(9) 0.5924(7) 0.6053(5) 0.056(3) Uani 1 1 d . . . . .
N6 N 0.5087(9) 0.8970(7) 0.7405(5) 0.054(3) Uani 1 1 d . . . . .
N16 N 0.4045(6) 0.4992(9) 0.8970(5) 0.057(3) Uani 1 1 d . . . . .
N13 N 0.0099(9) 0.3996(7) 0.7482(5) 0.055(3) Uani 1 1 d . . . . .
N7 N 0.5100(8) 0.9100(8) 0.5978(5) 0.055(3) Uani 1 1 d . . . . .
N8 N 0.6364(8) 1.0090(9) 0.6785(5) 0.062(3) Uani 1 1 d . . . . .
N10 N 0.8975(7) 1.0064(9) 0.7543(5) 0.056(3) Uani 1 1 d . . . . .
N15 N 0.0091(8) 0.1350(9) 0.8202(5) 0.061(3) Uani 1 1 d . . . . .
N1 N 0.1346(6) 0.5115(7) 0.6848(5) 0.050(3) Uani 1 1 d . . . . .
N4 N 0.5139(7) 0.6366(7) 0.8185(5) 0.048(3) Uani 1 1 d . . . . .
N3 N 0.3992(7) 0.5120(9) 0.7580(5) 0.056(3) Uani 1 1 d . . . . .
N18 N 0.4114(6) 0.4884(8) 1.1013(5) 0.049(3) Uani 1 1 d . . . . .
C1 C 0.0182(9) 0.6164(8) 0.5574(7) 0.049(3) Uani 1 1 d . . . . .
C2 C 0.0096(9) 0.3441(8) 0.7819(6) 0.046(3) Uani 1 1 d . . . . .
C12 C 0.8434(8) 1.0122(10) 0.7211(6) 0.053(3) Uani 1 1 d . . . . .
C11 C 0.7090(7) 1.0130(9) 0.6818(5) 0.044(3) Uani 1 1 d . . . . .
N14 N 0.0082(11) 0.2887(9) 0.8271(5) 0.079(4) Uani 1 1 d . . . . .
C4 C 0.2061(10) 0.5201(8) 0.6861(6) 0.050(3) Uani 1 1 d . . . . .
N9 N 0.7866(8) 1.0175(12) 0.6751(6) 0.085(5) Uani 1 1 d . . . . .
C3 C 0.0109(9) 0.2071(9) 0.8190(5) 0.045(3) Uani 1 1 d . . . . .
C8 C 0.5207(8) 0.7079(10) 0.8144(6) 0.051(4) Uani 1 1 d . . . . .
N2 N 0.2905(7) 0.5278(10) 0.6779(6) 0.072(4) Uani 1 1 d . . . . .
C9 C 0.5200(8) 0.8425(9) 0.7737(6) 0.046(3) Uani 1 1 d . . . . .
N5 N 0.5343(10) 0.7876(7) 0.8190(6) 0.069(4) Uani 1 1 d . . . . .
N11 N 0.0396(11) 0.6543(8) 0.5056(6) 0.082(4) Uani 1 1 d . U . A 1
C10 C 0.5219(9) 0.8830(7) 0.5476(6) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.3436(8) 0.5164(9) 0.7232(7) 0.050(3) Uani 1 1 d . . . . .
N60 N 0.2228(8) 0.2568(8) 0.1326(6) 0.057(3) Uani 1 1 d . . . . .
C61 C 0.2637(15) 0.2513(12) 0.2469(10) 0.091(8) Uani 1 1 d . . . . .
H61A H 0.3070 0.2070 0.2451 0.109 Uiso 1 1 calc R . . B 1
H61B H 0.2920 0.3048 0.2370 0.109 Uiso 1 1 calc R . . B 1
C60 C 0.2019(10) 0.2341(12) 0.1964(9) 0.076(5) Uani 1 1 d . . . C 1
H60A H 0.1896 0.1734 0.1970 0.091 Uiso 1 1 calc R . . C 1
H60B H 0.1492 0.2634 0.2072 0.091 Uiso 1 1 calc R . . C 1
C66 C 0.2983(16) 0.1115(14) 0.1176(12) 0.117(9) Uani 1 1 d . . . . .
H66A H 0.3011 0.0983 0.1622 0.141 Uiso 1 1 calc R . . . .
H66B H 0.2442 0.0900 0.1017 0.141 Uiso 1 1 calc R . . . .
N40 N 0.2564(8) 0.2749(8) 0.6310(6) 0.054(3) Uani 1 1 d . . . . .
C63B C 0.274(3) 0.255(3) 0.369(2) 0.055(11) Uiso 0.3333 1 d . . . C 2
H63A H 0.2555 0.2892 0.4039 0.083 Uiso 0.3333 1 calc GR . . C 2
H63B H 0.3212 0.2830 0.3482 0.083 Uiso 0.3333 1 calc GR . . C 2
H63C H 0.2918 0.2000 0.3834 0.083 Uiso 0.3333 1 calc GR . . C 2
C62A C 0.237(2) 0.256(2) 0.3060(15) 0.080(10) Uani 0.67 1 d . . . C 1
H62A H 0.1907 0.2158 0.3120 0.096 Uiso 0.67 1 calc R . . C 1
H62B H 0.2145 0.3131 0.3134 0.096 Uiso 0.67 1 calc R . . C 1
C48 C 0.2275(12) 0.3518(10) 0.5914(6) 0.067(4) Uani 1 1 d . . . . .
H48A H 0.2581 0.4020 0.6059 0.080 Uiso 1 1 calc R . . . .
H48B H 0.1671 0.3615 0.5992 0.080 Uiso 1 1 calc R . . . .
C70 C 0.1537(17) 0.240(2) 0.0235(9) 0.132(10) Uani 1 1 d . . . . .
H70C H 0.2043 0.2123 0.0069 0.158 Uiso 0.7 1 calc R . . D 2
H70D H 0.1572 0.3008 0.0140 0.158 Uiso 0.7 1 calc R . . D 2
H70A H 0.1811 0.1894 0.0068 0.158 Uiso 0.3333 1 calc R . . E 1
H70B H 0.1946 0.2864 0.0183 0.158 Uiso 0.3333 1 calc R . . E 1
C40 C 0.2320(11) 0.2992(10) 0.6980(6) 0.058(4) Uani 1 1 d . . . . .
H40A H 0.2601 0.3525 0.7087 0.070 Uiso 1 1 calc R . . . .
H40B H 0.1708 0.3092 0.6996 0.070 Uiso 1 1 calc R . . . .
C42 C 0.2425(17) 0.267(2) 0.8108(11) 0.155(13) Uani 1 1 d . . . . .
H42C H 0.2781 0.3176 0.8119 0.186 Uiso 0.54(9) 1 calc R . . F 2
H42D H 0.1841 0.2877 0.8106 0.186 Uiso 0.54(9) 1 calc R . . F 2
H42A H 0.1861 0.2918 0.8157 0.186 Uiso 0.46(9) 1 calc R . . F 1
H42B H 0.2853 0.3096 0.8210 0.186 Uiso 0.46(9) 1 calc R . . F 1
C69 C 0.1467(9) 0.2266(13) 0.0911(7) 0.071(5) Uani 1 1 d . . . . .
H69A H 0.1386 0.1659 0.0983 0.085 Uiso 1 1 calc R . . . .
H69B H 0.0955 0.2554 0.1057 0.085 Uiso 1 1 calc R . . . .
C65 C 0.3004(9) 0.2111(13) 0.1091(8) 0.075(5) Uani 1 1 d . . . . .
H65A H 0.3501 0.2333 0.1310 0.090 Uiso 1 1 calc R . . . .
H65B H 0.3075 0.2238 0.0646 0.090 Uiso 1 1 calc R . . . .
C53 C 0.4065(13) 0.3305(16) 0.6458(15) 0.123(9) Uani 1 1 d . . . . .
H53C H 0.3759 0.3800 0.6616 0.148 Uiso 0.5 1 calc R . . G 2
H53D H 0.4474 0.3109 0.6771 0.148 Uiso 0.5 1 calc R . . G 2
H53A H 0.3896 0.3837 0.6259 0.148 Uiso 0.5 1 calc R . . H 1
H53B H 0.4002 0.3377 0.6911 0.148 Uiso 0.5 1 calc R . . H 1
C50A C 0.224(5) 0.411(4) 0.479(3) 0.069(12) Uani 0.3333 1 d . . . I 1
H50A H 0.1641 0.4076 0.4683 0.083 Uiso 0.3333 1 calc R . . I 1
H50B H 0.2557 0.3990 0.4403 0.083 Uiso 0.3333 1 calc R . . I 1
C52 C 0.3472(12) 0.2604(10) 0.6241(9) 0.075(5) Uani 1 1 d . . . . .
H52A H 0.3587 0.2495 0.5798 0.090 Uiso 1 1 calc R . . . .
H52B H 0.3616 0.2088 0.6471 0.090 Uiso 1 1 calc R . . . .
C45 C 0.1164(12) 0.1987(15) 0.6157(11) 0.099(7) Uani 1 1 d . . . . .
H45A H 0.0957 0.2505 0.5956 0.119 Uiso 1 1 calc R . . . .
H45B H 0.1014 0.2022 0.6600 0.119 Uiso 1 1 calc R . . . .
C55B C 0.532(3) 0.335(4) 0.585(2) 0.098(17) Uiso 0.52(6) 1 d . . . J 2
H55A H 0.5597 0.3491 0.6236 0.147 Uiso 0.52(6) 1 calc GR . . J 2
H55B H 0.5521 0.3721 0.5519 0.147 Uiso 0.52(6) 1 calc GR . . J 2
H55C H 0.5450 0.2767 0.5737 0.147 Uiso 0.52(6) 1 calc GR . . J 2
C47 C -0.0113(16) 0.1286(18) 0.5940(14) 0.132(10) Uani 1 1 d . . . . .
H47A H -0.0228 0.1531 0.6347 0.198 Uiso 1 1 calc GR . . . .
H47B H -0.0373 0.0731 0.5915 0.198 Uiso 1 1 calc GR . . . .
H47C H -0.0345 0.1648 0.5617 0.198 Uiso 1 1 calc GR . . . .
C50B C 0.1906(19) 0.433(4) 0.492(2) 0.15(2) Uani 0.67 1 d . . . I 2
H50C H 0.1611 0.4270 0.4516 0.176 Uiso 0.67 1 calc R . . I 2
H50D H 0.1593 0.4665 0.5223 0.176 Uiso 0.67 1 calc R . . I 2
C49 C 0.2411(18) 0.3430(14) 0.5198(9) 0.110(8) Uani 1 1 d . . . . .
H49A H 0.3003 0.3267 0.5134 0.132 Uiso 1 1 calc R . . I 1
H49B H 0.2064 0.2952 0.5058 0.132 Uiso 1 1 calc R . . I 1
C44 C 0.2141(12) 0.1975(11) 0.6106(11) 0.087(6) Uani 1 1 d . . . . .
H44A H 0.2357 0.1502 0.6355 0.104 Uiso 1 1 calc R . . . .
H44B H 0.2295 0.1868 0.5669 0.104 Uiso 1 1 calc R . . . .
C54B C 0.441(3) 0.344(3) 0.592(3) 0.127(16) Uani 0.5 1 d . . . J 2
H54A H 0.4270 0.4022 0.5791 0.152 Uiso 0.5 1 calc R . . J 2
H54B H 0.4144 0.3064 0.5614 0.152 Uiso 0.5 1 calc R . . J 2
C72 C 0.000(2) 0.246(3) 0.0012(11) 0.184(15) Uani 1 1 d . . . . .
H72D H -0.0437 0.2149 0.0231 0.277 Uiso 0.67 1 calc GR . . K 2
H72E H -0.0215 0.2659 -0.0384 0.277 Uiso 0.67 1 calc GR . . K 2
H72F H 0.0179 0.2938 0.0264 0.277 Uiso 0.67 1 calc GR . . K 2
H72A H 0.0008 0.1928 0.0239 0.277 Uiso 0.3333 1 calc GR . . L 1
H72B H -0.0409 0.2429 -0.0323 0.277 Uiso 0.3333 1 calc GR . . L 1
H72C H -0.0148 0.2914 0.0295 0.277 Uiso 0.3333 1 calc GR . . L 1
C76 C 0.385(3) 0.0284(19) -0.080(2) 0.24(2) Uani 1 1 d . . . . .
H76A H 0.3565 0.0322 -0.0401 0.354 Uiso 1 1 calc GR . . . .
H76B H 0.4080 0.0832 -0.0913 0.354 Uiso 1 1 calc GR . . . .
H76C H 0.4299 -0.0129 -0.0779 0.354 Uiso 1 1 calc GR . . . .
C46 C 0.0684(18) 0.1217(14) 0.5865(14) 0.126(10) Uani 1 1 d . . . . .
H46A H 0.0812 0.1184 0.5418 0.151 Uiso 1 1 calc R . . . .
H46B H 0.0881 0.0693 0.6061 0.151 Uiso 1 1 calc R . . . .
C73 C 0.2420(13) 0.3484(12) 0.1227(10) 0.087(6) Uani 1 1 d . . . . .
H73A H 0.2943 0.3621 0.1451 0.105 Uiso 1 1 calc R . . . .
H73B H 0.2526 0.3577 0.0781 0.105 Uiso 1 1 calc R . . . .
C75 C 0.1875(17) 0.498(2) 0.1364(16) 0.177(16) Uani 1 1 d . . . . .
H75A H 0.2453 0.5112 0.1231 0.212 Uiso 1 1 calc R . . . .
H75B H 0.1761 0.5264 0.1761 0.212 Uiso 1 1 calc R . . . .
C71B C 0.064(4) 0.197(4) -0.008(2) 0.184(15) Uani 0.67 1 d . . . M 2
H71A H 0.0716 0.1891 -0.0533 0.221 Uiso 0.67 1 calc R . . M 2
H71B H 0.0529 0.1417 0.0105 0.221 Uiso 0.67 1 calc R . . M 2
C74 C 0.1765(17) 0.4064(16) 0.1428(13) 0.118(9) Uani 1 1 d . . . . .
H74A H 0.1658 0.3950 0.1871 0.142 Uiso 1 1 calc R . . . .
H74B H 0.1247 0.3913 0.1202 0.142 Uiso 1 1 calc R . . . .
C13 C 0.3843(9) 0.4851(14) 1.0518(7) 0.077(6) Uani 1 1 d . . . . .
C14 C 0.3831(8) 0.4848(14) 0.9458(7) 0.070(5) Uani 1 1 d . . . . .
N17 N 0.3483(8) 0.4588(11) 0.9980(5) 0.076(4) Uani 1 1 d . . . . .
C43A C 0.252(2) 0.233(3) 0.869(2) 0.078(16) Uiso 0.54(9) 1 d . . . F 2
H43A H 0.2744 0.1765 0.8657 0.117 Uiso 0.54(9) 1 calc GR . . F 2
H43B H 0.1971 0.2314 0.8896 0.117 Uiso 0.54(9) 1 calc GR . . F 2
H43C H 0.2902 0.2682 0.8932 0.117 Uiso 0.54(9) 1 calc GR . . F 2
C68 C 0.3642(15) -0.0267(17) 0.0998(15) 0.149(13) Uani 1 1 d . . . . .
H68A H 0.4144 -0.0544 0.0837 0.224 Uiso 1 1 calc GR . . . .
H68B H 0.3143 -0.0510 0.0805 0.224 Uiso 1 1 calc GR . . . .
H68C H 0.3613 -0.0346 0.1447 0.224 Uiso 1 1 calc GR . . . .
C67 C 0.3682(15) 0.0671(16) 0.0851(14) 0.121(9) Uani 1 1 d . . . . .
H67A H 0.4227 0.0902 0.0989 0.145 Uiso 1 1 calc R . . . .
H67B H 0.3634 0.0758 0.0400 0.145 Uiso 1 1 calc R . . . .
C51B C 0.285(4) 0.447(4) 0.489(3) 0.103(9) Uiso 0.37(3) 1 d . . . I 2
H51A H 0.3101 0.4869 0.5186 0.124 Uiso 0.37(3) 1 calc R . . I 2
H51B H 0.3119 0.4470 0.4473 0.124 Uiso 0.37(3) 1 calc R . . I 2
C54A C 0.498(3) 0.314(2) 0.631(3) 0.127(16) Uani 0.5 1 d . . . J 1
H54C H 0.5025 0.2698 0.5990 0.152 Uiso 0.5 1 calc R . . J 1
H54D H 0.5273 0.2934 0.6688 0.152 Uiso 0.5 1 calc R . . J 1
C41 C 0.2546(14) 0.2337(15) 0.7471(8) 0.089(8) Uani 1 1 d . . . . .
H41A H 0.2191 0.1835 0.7413 0.107 Uiso 1 1 calc R . . . .
H41B H 0.3138 0.2167 0.7417 0.107 Uiso 1 1 calc R . . . .
C62B C 0.204(4) 0.246(5) 0.324(3) 0.069(12) Uani 0.3333 1 d . U . C 2
H62C H 0.1625 0.2915 0.3281 0.083 Uiso 0.3333 1 calc R . . C 2
H62D H 0.1751 0.1910 0.3293 0.083 Uiso 0.3333 1 calc R . . C 2
C71A C 0.078(4) 0.261(7) -0.023(4) 0.15(4) Uani 0.3333 1 d . . . M 1
H71C H 0.0820 0.3204 -0.0354 0.176 Uiso 0.3333 1 calc R . . M 1
H71D H 0.0853 0.2265 -0.0609 0.176 Uiso 0.3333 1 calc R . . M 1
C63A C 0.315(3) 0.236(3) 0.360(2) 0.125(14) Uiso 0.67 1 d . . . C 1
H63D H 0.3182 0.1754 0.3673 0.188 Uiso 0.67 1 calc GR . . C 1
H63E H 0.3009 0.2643 0.3990 0.188 Uiso 0.67 1 calc GR . . C 1
H63F H 0.3685 0.2565 0.3447 0.188 Uiso 0.67 1 calc GR . . C 1
C55A C 0.541(3) 0.397(3) 0.607(2) 0.091(17) Uiso 0.48(6) 1 d . . . J 1
H55D H 0.5218 0.4098 0.5654 0.137 Uiso 0.48(6) 1 calc GR . . J 1
H55E H 0.6021 0.3904 0.6073 0.137 Uiso 0.48(6) 1 calc GR . . J 1
H55F H 0.5260 0.4438 0.6350 0.137 Uiso 0.48(6) 1 calc GR . . J 1
C43B C 0.253(3) 0.188(5) 0.852(3) 0.09(2) Uiso 0.46(9) 1 d . . . F 1
H43D H 0.3123 0.1755 0.8570 0.135 Uiso 0.46(9) 1 calc GR . . F 1
H43E H 0.2242 0.1407 0.8326 0.135 Uiso 0.46(9) 1 calc GR . . F 1
H43F H 0.2277 0.1990 0.8927 0.135 Uiso 0.46(9) 1 calc GR . . F 1
C51A C 0.243(3) 0.503(2) 0.4960(15) 0.103(9) Uiso 0.63(3) 1 d . . . I 1
H51C H 0.2212 0.5396 0.4635 0.155 Uiso 0.63(3) 1 calc GR . . I 1
H51D H 0.3032 0.5107 0.5003 0.155 Uiso 0.63(3) 1 calc GR . . I 1
H51E H 0.2151 0.5162 0.5353 0.155 Uiso 0.63(3) 1 calc GR . . I 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N12 Fe1 N12 83.2(6) . 2_565 ?
N13 Fe1 N12 172.3(5) 2_565 2_565 ?
N13 Fe1 N12 90.1(4) 2_565 . ?
N13 Fe1 N12 172.3(5) . . ?
N13 Fe1 N12 90.1(4) . 2_565 ?
N13 Fe1 N13 96.8(6) 2_565 . ?
N13 Fe1 N1 88.5(5) . . ?
N13 Fe1 N1 89.6(5) . 2_565 ?
N13 Fe1 N1 89.6(5) 2_565 . ?
N13 Fe1 N1 88.5(5) 2_565 2_565 ?
N1 Fe1 N12 93.9(5) . 2_565 ?
N1 Fe1 N12 88.3(5) . . ?
N1 Fe1 N12 88.3(5) 2_565 2_565 ?
N1 Fe1 N12 93.9(5) 2_565 . ?
N1 Fe1 N1 177.0(6) . 2_565 ?
N6 Fe2 N6 96.6(6) . 2_675 ?
N7 Fe2 N6 89.9(4) 2_675 2_675 ?
N7 Fe2 N6 173.4(4) 2_675 . ?
N7 Fe2 N6 89.9(4) . . ?
N7 Fe2 N6 173.4(4) . 2_675 ?
N7 Fe2 N7 83.6(6) . 2_675 ?
N7 Fe2 N8 94.2(5) 2_675 . ?
N7 Fe2 N8 94.2(5) . 2_675 ?
N7 Fe2 N8 90.9(5) . . ?
N7 Fe2 N8 90.9(5) 2_675 2_675 ?
N8 Fe2 N6 88.5(5) . 2_675 ?
N8 Fe2 N6 87.0(5) . . ?
N8 Fe2 N6 87.0(5) 2_675 2_675 ?
N8 Fe2 N6 88.5(5) 2_675 . ?
N8 Fe2 N8 173.2(6) . 2_675 ?
N10 Fe3 N10 96.1(6) 2_775 . ?
N15 Fe3 N10 89.0(5) 1_665 2_775 ?
N15 Fe3 N10 89.4(5) 1_665 . ?
N15 Fe3 N10 89.4(5) 2_665 2_775 ?
N15 Fe3 N10 89.0(5) 2_665 . ?
N15 Fe3 N15 177.6(6) 2_665 1_665 ?
N15 Fe3 N18 93.3(5) 1_665 4_657 ?
N15 Fe3 N18 88.6(5) 1_665 3_567 ?
N15 Fe3 N18 88.6(5) 2_665 4_657 ?
N15 Fe3 N18 93.3(5) 2_665 3_567 ?
N18 Fe3 N10 172.3(4) 4_657 . ?
N18 Fe3 N10 91.2(4) 4_657 2_775 ?
N18 Fe3 N10 91.2(4) 3_567 . ?
N18 Fe3 N10 172.2(4) 3_567 2_775 ?
N18 Fe3 N18 81.6(5) 4_657 3_567 ?
N16 Fe4 N16 87.1(6) . 2_665 ?
N4 Fe4 N16 96.1(5) 2_665 2_665 ?
N4 Fe4 N16 87.5(5) 2_665 . ?
N4 Fe4 N16 87.5(5) . 2_665 ?
N4 Fe4 N16 96.1(5) . . ?
N4 Fe4 N4 175.0(6) . 2_665 ?
N3 Fe4 N16 172.4(5) 2_665 . ?
N3 Fe4 N16 87.6(4) 2_665 2_665 ?
N3 Fe4 N16 87.6(4) . . ?
N3 Fe4 N16 172.4(5) . 2_665 ?
N3 Fe4 N4 87.6(5) . . ?
N3 Fe4 N4 89.1(5) . 2_665 ?
N3 Fe4 N4 87.6(5) 2_665 2_665 ?
N3 Fe4 N4 89.1(5) 2_665 . ?
N3 Fe4 N3 98.2(6) . 2_665 ?
C1 N12 Fe1 153.6(12) . . ?
C9 N6 Fe2 174.0(13) . . ?
C14 N16 Fe4 152.1(11) . . ?
C2 N13 Fe1 175.1(13) . . ?
C10 N7 Fe2 159.5(11) . . ?
C11 N8 Fe2 179.4(13) . . ?
C12 N10 Fe3 177.0(13) . . ?
C3 N15 Fe3 177.6(13) . 1_445 ?
C4 N1 Fe1 178.0(11) . . ?
C8 N4 Fe4 178.0(11) . . ?
C5 N3 Fe4 178.2(13) . . ?
C13 N18 Fe3 161.3(10) . 3_467 ?
N12 C1 N11 172.1(14) . . ?
N13 C2 N14 171.5(14) . . ?
N10 C12 N9 172.1(15) . . ?
N8 C11 N9 169.9(14) . . ?
C3 N14 C2 124.4(12) . . ?
N1 C4 N2 170.9(15) . . ?
C11 N9 C12 125.3(13) . . ?
N15 C3 N14 170.3(15) . . ?
N4 C8 N5 170.2(16) . . ?
C5 N2 C4 122.0(13) . . ?
N6 C9 N5 171.4(15) . . ?
C8 N5 C9 124.1(13) . . ?
C1 N11 C10 118.4(12) . 3_466 ?
N7 C10 N11 173.5(14) . 3_566 ?
N3 C5 N2 170.1(15) . . ?
C60 N60 C69 106.5(11) . . ?
C60 N60 C65 112.3(14) . . ?
C60 N60 C73 114.8(14) . . ?
C65 N60 C69 106.7(12) . . ?
C73 N60 C69 111.8(13) . . ?
C73 N60 C65 104.5(13) . . ?
C62A C61 C60 120(2) . . ?
N60 C60 C61 119.5(15) . . ?
C67 C66 C65 113.7(18) . . ?
C40 N40 C48 103.9(10) . . ?
C52 N40 C48 110.9(13) . . ?
C52 N40 C40 112.4(12) . . ?
C52 N40 C44 106.7(12) . . ?
C44 N40 C48 111.0(12) . . ?
C44 N40 C40 112.0(14) . . ?
C61 C62A C63A 114(3) . . ?
N40 C48 C49 115.4(13) . . ?
C69 C70 C71B 106(3) . . ?
C69 C70 C71A 126(3) . . ?
C41 C40 N40 114.7(13) . . ?
C43A C42 C41 134(4) . . ?
C41 C42 C43B 103(4) . . ?
C70 C69 N60 117.1(15) . . ?
N60 C65 C66 114.8(15) . . ?
C54B C53 C52 96(3) . . ?
C54A C53 C52 114(3) . . ?
C49 C50A C51A 123(5) . . ?
N40 C52 C53 117.3(14) . . ?
C44 C45 C46 116(2) . . ?
C51B C50B C49 72(3) . . ?
C48 C49 C50B 102(2) . . ?
C48 C49 C51B 109(3) . . ?
C50A C49 C48 121(3) . . ?
C50B C49 C51B 49(2) . . ?
N40 C44 C45 115.1(15) . . ?
C53 C54B C55B 119(5) . . ?
C47 C46 C45 111(2) . . ?
C74 C73 N60 115.2(17) . . ?
C74 C75 C76 105(3) . 4 ?
C72 C71B C70 110(5) . . ?
C73 C74 C75 121(2) . . ?
N18 C13 N17 164(2) . . ?
N16 C14 N17 169.7(18) . . ?
C14 N17 C13 116.9(13) . . ?
C66 C67 C68 110(2) . . ?
C50B C51B C49 60(4) . . ?
C53 C54A C55A 109(3) . . ?
C42 C41 C40 112(2) . . ?
C63B C62B C61 101(4) . . ?
C72 C71A C70 114(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N12 2.201(11) . ?
Fe1 N12 2.201(11) 2_565 ?
Fe1 N13 2.132(11) . ?
Fe1 N13 2.132(11) 2_565 ?
Fe1 N1 2.135(10) . ?
Fe1 N1 2.135(10) 2_565 ?
Fe2 N6 2.188(10) . ?
Fe2 N6 2.188(10) 2_675 ?
Fe2 N7 2.148(11) 2_675 ?
Fe2 N7 2.148(11) . ?
Fe2 N8 2.163(13) . ?
Fe2 N8 2.164(13) 2_675 ?
Fe3 N10 2.181(11) . ?
Fe3 N10 2.181(11) 2_775 ?
Fe3 N15 2.139(14) 2_665 ?
Fe3 N15 2.139(14) 1_665 ?
Fe3 N18 2.160(10) 4_657 ?
Fe3 N18 2.160(10) 3_567 ?
Fe4 N16 2.190(11) 2_665 ?
Fe4 N16 2.190(11) . ?
Fe4 N4 2.172(11) . ?
Fe4 N4 2.172(11) 2_665 ?
Fe4 N3 2.122(12) 2_665 ?
Fe4 N3 2.122(12) . ?
N12 C1 1.134(16) . ?
N6 C9 1.131(16) . ?
N16 C14 1.122(17) . ?
N13 C2 1.136(16) . ?
N7 C10 1.172(16) . ?
N8 C11 1.150(16) . ?
N10 C12 1.115(16) . ?
N15 Fe3 2.139(14) 1_445 ?
N15 C3 1.141(18) . ?
N1 C4 1.137(17) . ?
N4 C8 1.136(18) . ?
N3 C5 1.153(16) . ?
N18 Fe3 2.160(10) 3_467 ?
N18 C13 1.144(17) . ?
C1 N11 1.307(18) . ?
C2 N14 1.303(17) . ?
C12 N9 1.335(17) . ?
C11 N9 1.236(17) . ?
N14 C3 1.30(2) . ?
C4 N2 1.351(19) . ?
C8 N5 1.28(2) . ?
N2 C5 1.296(17) . ?
C9 N5 1.322(18) . ?
N11 C10 1.312(17) 3_466 ?
C10 N11 1.312(17) 3_566 ?
N60 C60 1.45(2) . ?
N60 C69 1.569(19) . ?
N60 C65 1.51(2) . ?
N60 C73 1.49(2) . ?
C61 C60 1.48(2) . ?
C61 C62A 1.33(4) . ?
C61 C62B 1.91(6) . ?
C66 C65 1.58(3) . ?
C66 C67 1.48(3) . ?
N40 C48 1.551(19) . ?
N40 C40 1.535(17) . ?
N40 C52 1.46(2) . ?
N40 C44 1.46(2) . ?
C63B C62B 1.47(8) . ?
C62A C63A 1.72(5) . ?
C48 C49 1.56(2) . ?
C70 C69 1.47(2) . ?
C70 C71B 1.72(7) . ?
C70 C71A 1.59(7) . ?
C40 C41 1.52(2) . ?
C42 C43A 1.36(5) . ?
C42 C41 1.47(3) . ?
C42 C43B 1.53(6) . ?
C53 C52 1.53(3) . ?
C53 C54B 1.31(5) . ?
C53 C54A 1.51(5) . ?
C50A C49 1.41(6) . ?
C50A C51A 1.53(8) . ?
C45 C44 1.55(3) . ?
C45 C46 1.57(3) . ?
C55B C54B 1.45(6) . ?
C47 C46 1.27(3) . ?
C50B C49 1.74(6) . ?
C50B C51B 1.51(7) . ?
C49 C51B 1.91(7) . ?
C72 C71B 1.28(5) . ?
C72 C71A 1.36(6) . ?
C76 C75 1.73(4) 4_545 ?
C73 C74 1.45(3) . ?
C75 C76 1.73(4) 4 ?
C75 C74 1.46(4) . ?
C13 N17 1.35(2) . ?
C14 N17 1.31(2) . ?
C68 C67 1.52(4) . ?
C54A C55A 1.57(6) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.93(3)
2 0.07(3)
