#------------------------------------------------------------------------------
#$Date: 2024-10-02 00:54:04 +0200 (Wed 02 de Oct de 2024) $
#$Revision: 294973 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/71/7717128.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_7717128
loop_
_publ_author_name
'Khrizanforov, Mikhail'
'Nailieva, Farida F.'
'Ivshin, Kamil'
'Zagidullin, Almaz'
'Samorodnova, Anastasiia P.'
'Shekurov, Ruslan Petrovich'
'Milyukova, Polina'
'Laskin, Artem'
'Novikov, Alexander S.'
'Vasili, Miluykov'
_publ_section_title
;
 Ugi's amine based coordination polymers as a synergistic catalysts for
 electrocatalytic reduction of carbon dioxide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D4DT01181C
_journal_year                    2024
_chemical_formula_moiety         'C32 H31 Co Fe N5 O4 P2'
_chemical_formula_sum            'C32 H31 Co Fe N5 O4 P2'
_chemical_formula_weight         726.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.368(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9939(16)
_cell_length_b                   11.4106(9)
_cell_length_c                   21.1115(16)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.64
_cell_volume                     4606.8(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2018.1-0'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22119
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.823
_diffrn_reflns_theta_min         1.785
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.609282
_exptl_absorpt_correction_T_min  0.211800
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1373 before and 0.0882 after correction.
 
For component 2:
 wR2(int) was 0.1454 before and 0.0980 after correction.
 The Ratio of minimum to maximum transmission is 0.69.

Final HKLF 4 output contains 112234 reflections, Rint = 0.1119
 (52051 with I > 3sig(I), Rint = 0.0807)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.202
_refine_diff_density_max         3.155
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.320
_refine_ls_extinction_coef       0.058(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   2.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         22119
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      2.292
_refine_ls_R_factor_all          0.2297
_refine_ls_R_factor_gt           0.1947
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5237
_refine_ls_wR_factor_ref         0.5443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16030
_reflns_number_total             22119
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01181c2.cif
_cod_data_source_block           zag001_12345
_cod_database_code               7717128
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.454(4)
 0.546(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C17-C16
 1.29 with sigma of 0.002
 C15-C17
 2.17 with sigma of 0.005
 C16-C18
 2.17 with sigma of 0.005
 C16-C15
 1.43 with sigma of 0.01
 C18-C17
 1.43 with sigma of 0.01
 C14-C15
 1.43 with sigma of 0.01
 C14-C18
 1.43 with sigma of 0.01
 C16-C17
 1.42 with sigma of 0.002
 C15-C16
 1.42 with sigma of 0.002
 C15-C18
 2.34 with sigma of 0.005
 C20-C21
 2.47 with sigma of 0.005
 N19-C20
 1.51 with sigma of 0.005
 N19-C21
 1.51 with sigma of 0.005
 C10-C9 \\sim C11-C10
 with sigma of 0.005
 C13-C9 \\sim C12-C13
 with sigma of 0.005
4. Restrained planarity
 C14, C15, C16, C17, C18
 with sigma of 0.005
 C9, C10, C11, C12, C13
 with sigma of 0.005
5. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.003 within 2A
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.003 within 2A
N19 \\sim C13: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.002 within 2A
P2: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.003 within
2A
P1 \\sim O1: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.004 within 2A
C2 \\sim C3 \\sim C4: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.004 within 2A
Uanis(Co1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(N5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.003
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.004
Uanis(N1) = Uanis(N5)
Uanis(C3) = Uanis(C30)
Uanis(C8) = Uanis(C25)
Uanis(N5) = Uanis(N1) = Uanis(N22) = Uanis(N28)
Uanis(C23) = Uanis(C24) = Uanis(C26) = Uanis(C27)
Uanis(C21) = Uanis(C20)
Uanis(C40) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C41) = Uanis(C39) =
Uanis(N38)
Uanis(C33) = Uanis(C30) = Uanis(C31) = Uanis(C32) = Uanis(C29)
Uanis(N38) = Uanis(N34)
6. Rigid body (RIGU) restrains
 C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N19, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Ternary CH refined with riding coordinates:
 N19(H19), C12(H12), C14(H14), C17(H17)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C15(H15), C16(H16),
 C18(H18), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32),
  C33(H33), C35(H35), C36(H36), C39(H39), C40(H40)
7.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Co1 Co 0.500000 0.28230(15) 0.750000 0.0147(5) Uani 1 2 d S TU P . .
Co2 Co 0.000000 0.2623(2) 0.250000 0.0301(6) Uani 1 2 d S T P . .
Fe1 Fe 0.73772(16) 0.3240(3) 0.61952(17) 0.0937(11) Uani 1 1 d . . . . .
P1 P 0.59637(18) 0.3458(3) 0.65693(18) 0.0429(8) Uani 1 1 d . U . . .
P2 P 0.0898(5) 0.2552(9) 0.1448(5) 0.140(3) Uani 1 1 d . . . . .
O1 O 0.5601(4) 0.2822(7) 0.6966(4) 0.0299(14) Uani 1 1 d . U . . .
O2 O 0.5533(6) 0.3930(11) 0.5873(7) 0.077(3) Uani 1 1 d . . . . .
O3 O 0.0574(4) 0.2550(7) 0.1918(4) 0.0379(19) Uani 1 1 d . . . . .
O4 O 0.0728(10) 0.328(3) 0.0871(11) 0.209(16) Uani 1 1 d . . . . .
N1 N 0.500000 0.0911(9) 0.750000 0.0202(9) Uani 1 2 d S TU P . .
N5 N 0.500000 0.4685(10) 0.750000 0.0202(9) Uani 1 2 d S TU P . .
N19 N 0.6109(8) 0.1521(14) 0.5446(8) 0.099(4) Uani 1 1 d D U . . .
H19 H 0.585931 0.226876 0.524433 0.119 Uiso 1 1 calc R U . . .
N22 N 0.4054(4) 0.2769(7) 0.6533(4) 0.0202(9) Uani 1 1 d . . . . .
N28 N 0.0940(4) 0.2563(7) 0.3449(4) 0.0202(9) Uani 1 1 d . . . . .
N34 N 0.000000 0.4510(17) 0.250000 0.0569(15) Uani 1 2 d S T P . .
N38 N 0.000000 0.0633(16) 0.250000 0.0569(15) Uani 1 2 d S T P . .
C2 C 0.4724(6) 0.0283(11) 0.7877(6) 0.037(2) Uani 1 1 d . U . . .
H2 H 0.452317 0.069530 0.814076 0.045 Uiso 1 1 calc R U . . .
C3 C 0.4724(7) -0.0858(13) 0.7890(7) 0.0460(12) Uani 1 1 d . U . . .
H3 H 0.453379 -0.125032 0.816889 0.055 Uiso 1 1 calc R U . . .
C4 C 0.500000 -0.1528(15) 0.750000 0.037(3) Uani 1 2 d S TU P . .
C6 C 0.5079(7) 0.5394(10) 0.8066(6) 0.038(3) Uani 1 1 d . . . . .
H6 H 0.512313 0.500127 0.847894 0.045 Uiso 1 1 calc R U . . .
C7 C 0.5099(8) 0.6506(11) 0.8092(6) 0.047(3) Uani 1 1 d . . . . .
H7 H 0.518307 0.687901 0.852129 0.057 Uiso 1 1 calc R U . . .
C8 C 0.500000 0.7224(14) 0.750000 0.0284(17) Uani 1 2 d S T P . .
C9 C 0.6669(10) 0.2501(16) 0.6530(10) 0.087(3) Uani 1 1 d D U . . .
C10 C 0.7386(8) 0.2495(17) 0.7149(12) 0.095(4) Uani 1 1 d D U . . .
H10 H 0.752527 0.283160 0.759781 0.114 Uiso 1 1 calc R U . . .
C11 C 0.7816(12) 0.1794(16) 0.6843(12) 0.100(4) Uani 1 1 d D U . . .
H11 H 0.829770 0.160216 0.707701 0.120 Uiso 1 1 calc R U . . .
C12 C 0.7429(11) 0.1522(17) 0.6242(12) 0.097(4) Uani 1 1 d D U . . .
H12 H 0.757786 0.102571 0.593655 0.117 Uiso 1 1 calc R U . . .
C13 C 0.6793(10) 0.1909(15) 0.6064(11) 0.093(3) Uani 1 1 d D U . . .
C14 C 0.7140(13) 0.4988(17) 0.5980(13) 0.175(8) Uani 1 1 d D U . . .
H14 H 0.682348 0.546252 0.612658 0.210 Uiso 1 1 calc R U . . .
C15 C 0.7864(12) 0.4771(18) 0.6388(10) 0.174(8) Uani 1 1 d D U . . .
H15 H 0.814259 0.504561 0.684360 0.208 Uiso 1 1 calc R U . . .
C16 C 0.8076(10) 0.4055(17) 0.5961(12) 0.172(8) Uani 1 1 d D U . . .
H16 H 0.853108 0.374925 0.607644 0.206 Uiso 1 1 calc R U . . .
C17 C 0.7507(13) 0.3889(16) 0.5360(11) 0.173(9) Uani 1 1 d D U . . .
H17 H 0.751188 0.338024 0.497629 0.207 Uiso 1 1 calc R U . . .
C18 C 0.6944(11) 0.440(2) 0.5333(11) 0.176(8) Uani 1 1 d D U . . .
H18 H 0.649441 0.439319 0.495777 0.211 Uiso 1 1 calc R U . . .
C20 C 0.5583(11) 0.080(2) 0.5593(11) 0.099(5) Uani 1 1 d D U . . .
H20A H 0.582730 0.018492 0.593100 0.148 Uiso 1 1 calc R U . . .
H20B H 0.525429 0.043674 0.516047 0.148 Uiso 1 1 calc R U . . .
H20C H 0.532694 0.130422 0.578227 0.148 Uiso 1 1 calc R U . . .
C21 C 0.6253(11) 0.097(2) 0.4871(10) 0.099(5) Uani 1 1 d D U . . .
H21A H 0.618300 0.155712 0.450784 0.148 Uiso 1 1 calc R U . . .
H21B H 0.593245 0.031366 0.467228 0.148 Uiso 1 1 calc R U . . .
H21C H 0.673638 0.068978 0.505673 0.148 Uiso 1 1 calc R U . . .
C23 C 0.3458(7) 0.3120(19) 0.6508(7) 0.070(3) Uani 1 1 d . . . . .
H23 H 0.344396 0.338273 0.692890 0.084 Uiso 1 1 calc R U . . .
C24 C 0.2829(7) 0.3145(18) 0.5905(7) 0.070(3) Uani 1 1 d . . . . .
H24 H 0.241114 0.342806 0.592318 0.084 Uiso 1 1 calc R U . . .
C25 C 0.2829(6) 0.2752(10) 0.5291(6) 0.0284(17) Uani 1 1 d . . . . .
C26 C 0.3487(7) 0.2446(18) 0.5320(7) 0.070(3) Uani 1 1 d . . . . .
H26 H 0.352297 0.219401 0.490692 0.084 Uiso 1 1 calc R U . . .
C27 C 0.4068(7) 0.2500(18) 0.5916(7) 0.070(3) Uani 1 1 d . . . . .
H27 H 0.450614 0.234330 0.590181 0.084 Uiso 1 1 calc R U . . .
C29 C 0.0989(7) 0.3122(13) 0.4051(7) 0.0460(12) Uani 1 1 d . . . . .
H29 H 0.057279 0.346136 0.404389 0.055 Uiso 1 1 calc R U . . .
C30 C 0.1556(7) 0.3228(13) 0.4629(7) 0.0460(12) Uani 1 1 d . . . . .
H30 H 0.154679 0.364529 0.501492 0.055 Uiso 1 1 calc R U . . .
C31 C 0.2187(8) 0.2703(14) 0.4666(7) 0.0460(12) Uani 1 1 d . . . . .
C32 C 0.2163(7) 0.2100(13) 0.4058(6) 0.0460(12) Uani 1 1 d . . . . .
H32 H 0.254187 0.165066 0.405278 0.055 Uiso 1 1 calc R U . . .
C33 C 0.1541(7) 0.2235(13) 0.3488(7) 0.0460(12) Uani 1 1 d . . . . .
H33 H 0.155719 0.205935 0.305459 0.055 Uiso 1 1 calc R U . . .
C35 C -0.0208(9) 0.5121(15) 0.2905(8) 0.0569(15) Uani 1 1 d . . . . .
H35 H -0.036510 0.469542 0.320048 0.068 Uiso 1 1 calc R U . . .
C36 C -0.0220(9) 0.6387(15) 0.2943(8) 0.0569(15) Uani 1 1 d . . . . .
H36 H -0.037127 0.677853 0.325392 0.068 Uiso 1 1 calc R U . . .
C37 C 0.000000 0.700(2) 0.250000 0.0569(15) Uani 1 2 d S T P . .
C39 C -0.0174(9) 0.0151(14) 0.1924(8) 0.0569(15) Uani 1 1 d . . . . .
H39 H -0.030681 0.059387 0.150813 0.068 Uiso 1 1 calc R U . . .
C40 C -0.0165(8) -0.1191(14) 0.1917(8) 0.0569(15) Uani 1 1 d . . . . .
H40 H -0.027856 -0.160638 0.149457 0.068 Uiso 1 1 calc R U . . .
C41 C 0.000000 -0.175(2) 0.250000 0.0569(15) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
O1 Co1 O1 180.0(4) 2_656 . ?
O1 Co1 N1 90.0(2) 2_656 . ?
O1 Co1 N1 90.0(2) . . ?
O1 Co1 N5 90.0(2) 2_656 . ?
O1 Co1 N5 90.0(2) . . ?
O1 Co1 N22 89.1(3) 2_656 . ?
O1 Co1 N22 90.9(3) . . ?
O1 Co1 N22 90.9(3) 2_656 2_656 ?
O1 Co1 N22 89.1(3) . 2_656 ?
N1 Co1 N22 88.4(2) . 2_656 ?
N1 Co1 N22 88.4(2) . . ?
N5 Co1 N1 180.0 . . ?
N5 Co1 N22 91.6(2) . 2_656 ?
N5 Co1 N22 91.6(2) . . ?
N22 Co1 N22 176.8(4) 2_656 . ?
O3 Co2 O3 175.3(5) 2 . ?
O3 Co2 N28 90.9(3) . . ?
O3 Co2 N28 90.9(3) 2 2 ?
O3 Co2 N28 88.9(3) 2 . ?
O3 Co2 N28 88.9(3) . 2 ?
O3 Co2 N34 92.3(2) . . ?
O3 Co2 N34 92.3(2) 2 . ?
O3 Co2 N38 87.7(2) 2 . ?
O3 Co2 N38 87.7(2) . . ?
N28 Co2 N28 176.3(4) 2 . ?
N28 Co2 N38 88.2(2) . . ?
N28 Co2 N38 88.2(2) 2 . ?
N34 Co2 N28 91.8(2) . . ?
N34 Co2 N28 91.8(2) . 2 ?
N34 Co2 N38 180.0 . . ?
C9 Fe1 C10 42.2(6) . . ?
C9 Fe1 C11 69.0(8) . . ?
C9 Fe1 C18 115.6(7) . . ?
C11 Fe1 C10 42.0(6) . . ?
C11 Fe1 C18 164.8(9) . . ?
C12 Fe1 C9 67.0(8) . . ?
C12 Fe1 C10 65.5(9) . . ?
C12 Fe1 C11 35.1(8) . . ?
C12 Fe1 C14 168.8(10) . . ?
C12 Fe1 C15 149.0(10) . . ?
C12 Fe1 C17 112.5(8) . . ?
C12 Fe1 C18 131.4(9) . . ?
C13 Fe1 C9 38.1(6) . . ?
C13 Fe1 C10 65.3(8) . . ?
C13 Fe1 C11 63.2(8) . . ?
C13 Fe1 C12 39.5(6) . . ?
C13 Fe1 C14 131.2(9) . . ?
C13 Fe1 C15 169.5(7) . . ?
C13 Fe1 C16 147.8(8) . . ?
C13 Fe1 C17 118.3(8) . . ?
C13 Fe1 C18 110.6(8) . . ?
C14 Fe1 C9 109.1(7) . . ?
C14 Fe1 C10 119.4(8) . . ?
C14 Fe1 C11 155.0(10) . . ?
C14 Fe1 C18 39.5(5) . . ?
C15 Fe1 C9 132.3(7) . . ?
C15 Fe1 C10 110.4(8) . . ?
C15 Fe1 C11 120.7(10) . . ?
C15 Fe1 C14 41.3(5) . . ?
C15 Fe1 C17 67.3(4) . . ?
C15 Fe1 C18 68.1(4) . . ?
C16 Fe1 C9 174.0(9) . . ?
C16 Fe1 C10 134.0(8) . . ?
C16 Fe1 C11 111.3(8) . . ?
C16 Fe1 C12 116.9(8) . . ?
C16 Fe1 C14 67.9(5) . . ?
C16 Fe1 C15 42.1(4) . . ?
C16 Fe1 C17 39.5(2) . . ?
C16 Fe1 C18 65.8(4) . . ?
C17 Fe1 C9 144.7(9) . . ?
C17 Fe1 C10 172.4(8) . . ?
C17 Fe1 C11 132.2(8) . . ?
C17 Fe1 C14 64.1(6) . . ?
C17 Fe1 C18 36.3(4) . . ?
C18 Fe1 C10 150.6(7) . . ?
O1 P1 C9 109.3(7) . . ?
O2 P1 O1 118.7(7) . . ?
O2 P1 C9 109.9(8) . . ?
O4 P2 O3 126.2(13) . . ?
P1 O1 Co1 151.4(5) . . ?
P2 O3 Co2 173.0(7) . . ?
C2 N1 Co1 121.6(7) 2_656 . ?
C2 N1 Co1 121.6(7) . . ?
C2 N1 C2 116.7(13) 2_656 . ?
C6 N5 Co1 125.5(6) 2_656 . ?
C6 N5 Co1 125.5(6) . . ?
C6 N5 C6 109.1(11) 2_656 . ?
C13 N19 H19 104.8 . . ?
C20 N19 H19 104.8 . . ?
C20 N19 C13 119.0(15) . . ?
C21 N19 H19 104.8 . . ?
C21 N19 C13 111.8(14) . . ?
C21 N19 C20 110.3(7) . . ?
C23 N22 Co1 121.4(7) . . ?
C23 N22 C27 115.8(10) . . ?
C27 N22 Co1 122.3(7) . . ?
C29 N28 Co2 122.0(7) . . ?
C33 N28 Co2 124.5(8) . . ?
C33 N28 C29 112.0(10) . . ?
C35 N34 Co2 122.2(10) . . ?
C35 N34 Co2 122.2(10) 2 . ?
C35 N34 C35 116(2) 2 . ?
C39 N38 Co2 116.3(11) 2 . ?
C39 N38 Co2 116.3(11) . . ?
C39 N38 C39 127(2) 2 . ?
N1 C2 H2 118.7 . . ?
C3 C2 N1 122.6(11) . . ?
C3 C2 H2 118.7 . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.8(12) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C3 114.3(17) 2_656 . ?
C3 C4 C8 122.8(8) . 1_545 ?
C3 C4 C8 122.8(8) 2_656 1_545 ?
N5 C6 H6 116.3 . . ?
C7 C6 N5 127.3(10) . . ?
C7 C6 H6 116.3 . . ?
C6 C7 H7 118.6 . . ?
C6 C7 C8 122.9(11) . . ?
C8 C7 H7 118.6 . . ?
C4 C8 C7 124.8(7) 1_565 . ?
C4 C8 C7 124.8(7) 1_565 2_656 ?
C7 C8 C7 110.4(14) . 2_656 ?
P1 C9 Fe1 118.1(9) . . ?
C10 C9 Fe1 72.6(9) . . ?
C10 C9 P1 118.8(14) . . ?
C13 C9 Fe1 63.8(9) . . ?
C13 C9 P1 138.1(16) . . ?
C13 C9 C10 102.0(15) . . ?
Fe1 C10 H10 130.2 . . ?
C9 C10 Fe1 65.1(9) . . ?
C9 C10 H10 129.7 . . ?
C9 C10 C11 100.6(18) . . ?
C11 C10 Fe1 66.2(10) . . ?
C11 C10 H10 129.7 . . ?
Fe1 C11 H11 127.4 . . ?
C10 C11 Fe1 71.8(9) . . ?
C10 C11 H11 125.9 . . ?
C12 C11 Fe1 66.5(11) . . ?
C12 C11 C10 108.2(19) . . ?
C12 C11 H11 125.9 . . ?
Fe1 C12 H12 124.0 . . ?
C11 C12 Fe1 78.5(12) . . ?
C11 C12 H12 124.0 . . ?
C11 C12 C13 112(2) . . ?
C13 C12 Fe1 67.6(9) . . ?
C13 C12 H12 124.0 . . ?
N19 C13 Fe1 131.9(13) . . ?
C9 C13 Fe1 78.1(11) . . ?
C9 C13 N19 112.1(15) . . ?
C9 C13 C12 117(2) . . ?
C12 C13 Fe1 72.9(10) . . ?
C12 C13 N19 128.9(18) . . ?
Fe1 C14 H14 125.9 . . ?
C15 C14 Fe1 66.3(9) . . ?
C15 C14 H14 125.9 . . ?
C18 C14 Fe1 72.9(9) . . ?
C18 C14 H14 125.9 . . ?
C18 C14 C15 108.2(10) . . ?
Fe1 C15 H15 123.3 . . ?
C14 C15 Fe1 72.4(9) . . ?
C14 C15 H15 127.7 . . ?
C16 C15 Fe1 68.4(6) . . ?
C16 C15 C14 104.6(7) . . ?
C16 C15 H15 127.7 . . ?
Fe1 C16 H16 122.6 . . ?
C15 C16 Fe1 69.5(7) . . ?
C15 C16 H16 126.6 . . ?
C17 C16 Fe1 73.0(9) . . ?
C17 C16 C15 106.9(4) . . ?
C17 C16 H16 126.6 . . ?
Fe1 C17 H17 122.8 . . ?
C16 C17 Fe1 67.5(9) . . ?
C16 C17 H17 122.8 . . ?
C18 C17 Fe1 76.0(7) . . ?
C18 C17 C16 114.4(6) . . ?
C18 C17 H17 122.8 . . ?
Fe1 C18 H18 129.1 . . ?
C14 C18 Fe1 67.6(8) . . ?
C14 C18 H18 127.1 . . ?
C17 C18 Fe1 67.7(6) . . ?
C17 C18 C14 105.9(7) . . ?
C17 C18 H18 127.1 . . ?
N19 C20 H20A 109.5 . . ?
N19 C20 H20B 109.5 . . ?
N19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N19 C21 H21A 109.5 . . ?
N19 C21 H21B 109.5 . . ?
N19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N22 C23 H23 117.4 . . ?
N22 C23 C24 125.1(11) . . ?
C24 C23 H23 117.4 . . ?
C23 C24 H24 120.6 . . ?
C25 C24 C23 118.9(12) . . ?
C25 C24 H24 120.6 . . ?
C24 C25 C26 115.2(11) . . ?
C24 C25 C31 120.8(12) . . ?
C26 C25 C31 124.1(11) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 C25 121.7(11) . . ?
C27 C26 H26 119.1 . . ?
N22 C27 H27 118.6 . . ?
C26 C27 N22 122.7(12) . . ?
C26 C27 H27 118.6 . . ?
N28 C29 H29 116.9 . . ?
C30 C29 N28 126.2(12) . . ?
C30 C29 H29 116.9 . . ?
C29 C30 H30 120.7 . . ?
C29 C30 C31 118.5(12) . . ?
C31 C30 H30 120.7 . . ?
C30 C31 C25 121.9(12) . . ?
C30 C31 C32 117.6(13) . . ?
C32 C31 C25 120.5(12) . . ?
C31 C32 H32 123.2 . . ?
C33 C32 C31 113.5(12) . . ?
C33 C32 H32 123.2 . . ?
N28 C33 C32 129.9(12) . . ?
N28 C33 H33 115.0 . . ?
C32 C33 H33 115.0 . . ?
N34 C35 H35 117.1 . . ?
N34 C35 C36 125.8(15) . . ?
C36 C35 H35 117.1 . . ?
C35 C36 H36 121.7 . . ?
C37 C36 C35 116.6(15) . . ?
C37 C36 H36 121.7 . . ?
C36 C37 C36 119(2) 2 . ?
C36 C37 C41 120.3(11) 2 1_565 ?
C36 C37 C41 120.3(11) . 1_565 ?
N38 C39 H39 121.6 . . ?
N38 C39 C40 116.9(15) . . ?
C40 C39 H39 121.6 . . ?
C39 C40 H40 120.5 . . ?
C41 C40 C39 118.9(15) . . ?
C41 C40 H40 120.5 . . ?
C40 C41 C37 119.5(12) 2 1_545 ?
C40 C41 C37 119.5(12) . 1_545 ?
C40 C41 C40 121(2) . 2 ?
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
Co1 O1 2.009(7) 2_656 ?
Co1 O1 2.009(7) . ?
Co1 N1 2.182(11) . ?
Co1 N5 2.124(11) . ?
Co1 N22 2.184(8) . ?
Co1 N22 2.184(8) 2_656 ?
Co2 O3 2.047(8) 2 ?
Co2 O3 2.047(8) . ?
Co2 N28 2.156(8) . ?
Co2 N28 2.156(8) 2 ?
Co2 N34 2.15(2) . ?
Co2 N38 2.271(19) . ?
Fe1 C9 2.072(19) . ?
Fe1 C10 2.18(2) . ?
Fe1 C11 2.10(2) . ?
Fe1 C12 1.96(2) . ?
Fe1 C13 1.90(2) . ?
Fe1 C14 2.06(2) . ?
Fe1 C15 1.98(2) . ?
Fe1 C16 1.964(15) . ?
Fe1 C17 2.032(15) . ?
Fe1 C18 2.13(2) . ?
P1 O1 1.527(7) . ?
P1 O2 1.474(12) . ?
P1 C9 1.869(19) . ?
P2 O3 1.415(10) . ?
P2 O4 1.393(18) . ?
N1 C2 1.365(12) 2_656 ?
N1 C2 1.365(12) . ?
N5 C6 1.396(13) 2_656 ?
N5 C6 1.396(13) . ?
N19 H19 1.0000 . ?
N19 C13 1.55(3) . ?
N19 C20 1.508(7) . ?
N19 C21 1.504(7) . ?
N22 C23 1.294(15) . ?
N22 C27 1.352(15) . ?
N28 C29 1.388(15) . ?
N28 C33 1.287(15) . ?
N34 C35 1.311(18) 2 ?
N34 C35 1.311(18) . ?
N38 C39 1.244(17) . ?
N38 C39 1.244(17) 2 ?
C2 H2 0.9500 . ?
C2 C3 1.30(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.410(16) . ?
C4 C8 1.42(2) 1_545 ?
C6 H6 0.9500 . ?
C6 C7 1.270(18) . ?
C7 H7 0.9500 . ?
C7 C8 1.436(15) . ?
C9 C10 1.53(2) . ?
C9 C13 1.306(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.53(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.23(3) . ?
C12 H12 1.0000 . ?
C12 C13 1.306(18) . ?
C14 H14 1.0000 . ?
C14 C15 1.426(13) . ?
C14 C18 1.419(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.416(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.351(2) . ?
C17 H17 1.0000 . ?
C17 C18 1.299(10) . ?
C18 H18 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23 0.9500 . ?
C23 C24 1.405(18) . ?
C24 H24 0.9500 . ?
C24 C25 1.371(16) . ?
C25 C26 1.402(17) . ?
C25 C31 1.45(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.345(18) . ?
C27 H27 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.313(19) . ?
C30 H30 0.9500 . ?
C30 C31 1.425(19) . ?
C31 C32 1.440(19) . ?
C32 H32 0.9500 . ?
C32 C33 1.371(19) . ?
C33 H33 0.9500 . ?
C35 H35 0.9500 . ?
C35 C36 1.45(2) . ?
C36 H36 0.9500 . ?
C36 C37 1.39(2) . ?
C37 C41 1.42(3) 1_565 ?
C39 H39 0.9500 . ?
C39 C40 1.53(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.301(19) . ?
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
Co1 N1 C2 C3 -179.3(10) . . . . ?
Co1 N5 C6 C7 178.1(12) . . . . ?
Co1 N22 C23 C24 178.2(16) . . . . ?
Co1 N22 C27 C26 178.9(16) . . . . ?
Co2 N28 C29 C30 -173.0(11) . . . . ?
Co2 N28 C33 C32 -176.1(12) . . . . ?
Co2 N34 C35 C36 179.5(12) . . . . ?
Co2 N38 C39 C40 179.0(10) . . . . ?
Fe1 C9 C10 C11 -57.3(7) . . . . ?
Fe1 C9 C13 N19 -130.7(14) . . . . ?
Fe1 C9 C13 C12 63.5(8) . . . . ?
Fe1 C10 C11 C12 -56.6(7) . . . . ?
Fe1 C11 C12 C13 -59.9(7) . . . . ?
Fe1 C12 C13 N19 130.5(17) . . . . ?
Fe1 C12 C13 C9 -66.4(8) . . . . ?
Fe1 C14 C15 C16 61.2(6) . . . . ?
Fe1 C14 C18 C17 -57.1(7) . . . . ?
Fe1 C15 C16 C17 63.9(9) . . . . ?
Fe1 C16 C17 C18 61.6(7) . . . . ?
Fe1 C17 C18 C14 57.0(8) . . . . ?
P1 C9 C10 Fe1 -113.0(11) . . . . ?
P1 C9 C10 C11 -170.3(14) . . . . ?
P1 C9 C13 Fe1 103.7(17) . . . . ?
P1 C9 C13 N19 -27(2) . . . . ?
P1 C9 C13 C12 167.3(19) . . . . ?
O1 P1 C9 Fe1 -168.3(8) . . . . ?
O1 P1 C9 C10 -83.6(11) . . . . ?
O1 P1 C9 C13 110.6(16) . . . . ?
O2 P1 O1 Co1 -71.7(13) . . . . ?
O2 P1 C9 Fe1 59.8(12) . . . . ?
O2 P1 C9 C10 144.5(11) . . . . ?
O2 P1 C9 C13 -21.3(19) . . . . ?
N1 C2 C3 C4 -1.3(19) . . . . ?
N5 C6 C7 C8 4(2) . . . . ?
N22 C23 C24 C25 1(3) . . . . ?
N28 C29 C30 C31 -2(2) . . . . ?
N34 C35 C36 C37 1(2) . . . . ?
N38 C39 C40 C41 2(2) . . . . ?
C2 N1 C2 C3 0.7(10) 2_656 . . . ?
C2 C3 C4 C3 0.6(10) . . . 2_656 ?
C2 C3 C4 C8 -179.4(10) . . . 1_545 ?
C6 N5 C6 C7 -1.9(12) 2_656 . . . ?
C6 C7 C8 C4 178.3(11) . . . 1_565 ?
C6 C7 C8 C7 -1.7(11) . . . 2_656 ?
C9 Fe1 C13 N19 109.1(18) . . . . ?
C9 Fe1 C13 C12 -123.5(19) . . . . ?
C9 P1 O1 Co1 161.2(11) . . . . ?
C9 C10 C11 Fe1 56.6(7) . . . . ?
C9 C10 C11 C12 0.02(15) . . . . ?
C10 Fe1 C13 N19 151.9(16) . . . . ?
C10 Fe1 C13 C9 42.7(9) . . . . ?
C10 Fe1 C13 C12 -80.8(14) . . . . ?
C10 C9 C13 Fe1 -63.6(7) . . . . ?
C10 C9 C13 N19 165.7(16) . . . . ?
C10 C9 C13 C12 -0.1(3) . . . . ?
C10 C11 C12 Fe1 59.9(7) . . . . ?
C10 C11 C12 C13 -0.1(3) . . . . ?
C11 Fe1 C13 N19 -161.3(17) . . . . ?
C11 Fe1 C13 C9 89.6(14) . . . . ?
C11 Fe1 C13 C12 -34.0(12) . . . . ?
C11 C12 C13 Fe1 66.5(8) . . . . ?
C11 C12 C13 N19 -163.0(19) . . . . ?
C11 C12 C13 C9 0.1(4) . . . . ?
C12 Fe1 C13 N19 -127(2) . . . . ?
C12 Fe1 C13 C9 123.5(19) . . . . ?
C13 C9 C10 Fe1 57.4(7) . . . . ?
C13 C9 C10 C11 0.02(14) . . . . ?
C14 Fe1 C13 N19 43.5(19) . . . . ?
C14 Fe1 C13 C9 -65.6(16) . . . . ?
C14 Fe1 C13 C12 170.8(13) . . . . ?
C14 C15 C16 Fe1 -63.9(9) . . . . ?
C14 C15 C16 C17 -0.01(16) . . . . ?
C15 Fe1 C13 N19 84(5) . . . . ?
C15 Fe1 C13 C9 -25(5) . . . . ?
C15 Fe1 C13 C12 -148(5) . . . . ?
C15 C14 C18 Fe1 57.0(7) . . . . ?
C15 C14 C18 C17 0.0(3) . . . . ?
C15 C16 C17 Fe1 -61.7(6) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C16 Fe1 C13 N19 -73(2) . . . . ?
C16 Fe1 C13 C9 177.5(15) . . . . ?
C16 Fe1 C13 C12 54(2) . . . . ?
C16 C17 C18 Fe1 -57.0(8) . . . . ?
C16 C17 C18 C14 0.0(4) . . . . ?
C17 Fe1 C13 N19 -35.6(17) . . . . ?
C17 Fe1 C13 C9 -144.7(12) . . . . ?
C17 Fe1 C13 C12 91.7(15) . . . . ?
C18 Fe1 C13 N19 3.5(16) . . . . ?
C18 Fe1 C13 C9 -105.6(12) . . . . ?
C18 Fe1 C13 C12 130.9(13) . . . . ?
C18 C14 C15 Fe1 -61.1(6) . . . . ?
C18 C14 C15 C16 0.02(15) . . . . ?
C20 N19 C13 Fe1 -150.4(14) . . . . ?
C20 N19 C13 C9 -56.7(18) . . . . ?
C20 N19 C13 C12 107.1(19) . . . . ?
C21 N19 C13 Fe1 79.1(18) . . . . ?
C21 N19 C13 C9 172.9(14) . . . . ?
C21 N19 C13 C12 -23(2) . . . . ?
C23 N22 C27 C26 -9(3) . . . . ?
C23 C24 C25 C26 -5(3) . . . . ?
C23 C24 C25 C31 176.7(16) . . . . ?
C24 C25 C26 C27 2(3) . . . . ?
C24 C25 C31 C30 10(2) . . . . ?
C24 C25 C31 C32 -168.7(15) . . . . ?
C25 C26 C27 N22 5(3) . . . . ?
C25 C31 C32 C33 -173.5(12) . . . . ?
C26 C25 C31 C30 -167.8(16) . . . . ?
C26 C25 C31 C32 13(2) . . . . ?
C27 N22 C23 C24 6(3) . . . . ?
C29 N28 C33 C32 18(2) . . . . ?
C29 C30 C31 C25 -178.2(12) . . . . ?
C29 C30 C31 C32 1(2) . . . . ?
C30 C31 C32 C33 7(2) . . . . ?
C31 C25 C26 C27 -179.6(17) . . . . ?
C31 C32 C33 N28 -18(2) . . . . ?
C33 N28 C29 C30 -6.3(19) . . . . ?
C35 N34 C35 C36 -0.5(12) 2 . . . ?
C35 C36 C37 C36 -0.4(10) . . . 2 ?
C35 C36 C37 C41 179.6(10) . . . 1_565 ?
C39 N38 C39 C40 -1.0(10) 2 . . . ?
C39 C40 C41 C37 179.0(10) . . . 1_545 ?
C39 C40 C41 C40 -1.0(10) . . . 2 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.454(4)
2 0.546(4)
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.304 0.000 954.5 199.9 ?
2 0.000 -0.564 0.500 954.5 199.9 ?
