#------------------------------------------------------------------------------
#$Date: 2021-01-02 05:19:15 +0200 (Sat, 02 Jan 2021) $
#$Revision: 260360 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/99/1559904.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_1559904
loop_
_publ_author_name
'Rajak, Sanil'
'Schott,  Olivier'
'Kaur,  Prabhjyot'
'Maris, Thierry'
'Hanan,  Garry S.'
'Duong, Adam'
_publ_section_title
;
 Design of a [FeFe] macrocyclic metallotecton for light-driven hydrogen
 evolution reaction
;
_journal_name_full               'International Journal Of Hydrogen Energy'
_journal_page_first              2699
_journal_page_last               2708
_journal_paper_doi               10.1016/j.ijhydene.2019.11.141
_journal_volume                  45
_journal_year                    2020
_chemical_formula_moiety
'C33 H37 Fe2 N24 O5 P2, 2(N O3), 3.25(C H4 O)'
_chemical_formula_sum            'C36.25 H50 Fe2 N26 O14.25 P2'
_chemical_formula_weight         1251.66
_chemical_name_systematic
;
(μ-dihydrogen phosphinato)-(μ-methyl phosphito)-tetrakis(6-(2-pyridyl)
-1,3,5-triazine-2,4-diamine)-di-iron dinitrate methanol solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.687(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6206(3)
_cell_length_b                   14.3962(4)
_cell_length_c                   19.5412(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.637
_cell_measurement_theta_min      3.339
_cell_volume                     2935.95(15)
_computing_cell_refinement
;
SAINT (2013) V8.38A; Integration Software for Single Crystal Data. 
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2013) V8.38A; Integration Software for Single Crystal Data. 
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.704
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.524
_exptl_absorpt_correction_T_max  0.4613
_exptl_absorpt_correction_T_min  0.3269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1236 before and 0.0660 after correction. 
The Ratio of minimum to maximum transmission is 0.7086. 
The λ/2 correction factor is Not present.'
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1291
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0055(5)
_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   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6753
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1110P)²+1.9273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6096
_reflns_number_total             6753
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            rm262.cif
_cod_data_source_block           rm262
_cod_database_code               1559904
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 '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
C1 C 0.9353(3) 0.4736(2) 0.69422(15) 0.0471(6) Uani 1 1 d . . . . .
H1 H 0.871346 0.480527 0.722009 0.057 Uiso 1 1 calc R . . . .
C2 C 1.0597(3) 0.4997(3) 0.72198(16) 0.0535(8) Uani 1 1 d . . . . .
H2 H 1.080570 0.523800 0.767955 0.064 Uiso 1 1 calc R . . . .
C3 C 1.1528(3) 0.4903(2) 0.68181(16) 0.0483(7) Uani 1 1 d . . . . .
H3 H 1.238715 0.508594 0.699316 0.058 Uiso 1 1 calc R . . . .
C4 C 1.1186(2) 0.4535(2) 0.61517(15) 0.0427(6) Uani 1 1 d . . . . .
H4 H 1.180968 0.445552 0.586537 0.051 Uiso 1 1 calc R . . . .
C5 C 0.9920(2) 0.42848(18) 0.59113(13) 0.0340(5) Uani 1 1 d . . . . .
C6 C 0.9507(2) 0.38666(18) 0.52093(12) 0.0329(5) Uani 1 1 d . . . . .
C7 C 0.7924(2) 0.32768(18) 0.43775(13) 0.0354(5) Uani 1 1 d . . . . .
C8 C 0.9996(2) 0.3250(2) 0.42349(13) 0.0394(5) Uani 1 1 d . . . . .
C9 C 0.7682(3) 0.1954(2) 0.59241(17) 0.0511(7) Uani 1 1 d . . . . .
H9 H 0.813996 0.207003 0.555876 0.061 Uiso 1 1 calc R . . . .
C10 C 0.7609(4) 0.1049(2) 0.61532(19) 0.0567(8) Uani 1 1 d . . . . .
H10 H 0.800133 0.055620 0.594628 0.068 Uiso 1 1 calc R . . . .
C11 C 0.6961(4) 0.0877(2) 0.66828(18) 0.0557(8) Uani 1 1 d . . . . .
H11 H 0.689269 0.026237 0.684942 0.067 Uiso 1 1 calc R . . . .
C12 C 0.6405(3) 0.1614(2) 0.69718(15) 0.0515(7) Uani 1 1 d . . . . .
H12 H 0.595361 0.151115 0.734146 0.062 Uiso 1 1 calc R . . . .
C13 C 0.6513(3) 0.25032(19) 0.67183(13) 0.0382(5) Uani 1 1 d . . . . .
C14 C 0.5934(2) 0.33234(19) 0.70043(13) 0.0366(5) Uani 1 1 d . . . . .
C15 C 0.4740(3) 0.3947(2) 0.77278(15) 0.0443(6) Uani 1 1 d . . . . .
C16 C 0.5631(2) 0.48842(19) 0.70177(13) 0.0370(5) Uani 1 1 d . . . . .
Fe1 Fe 0.70583(3) 0.40959(2) 0.57872(2) 0.03121(15) Uani 1 1 d . . . . .
N1 N 0.9013(2) 0.43900(16) 0.62995(11) 0.0365(4) Uani 1 1 d . . . . .
N2 N 0.82425(19) 0.37143(15) 0.50080(10) 0.0329(4) Uani 1 1 d . . . . .
N3 N 0.8778(2) 0.30115(17) 0.39854(11) 0.0385(5) Uani 1 1 d . . . . .
N4 N 1.0418(2) 0.36751(18) 0.48597(11) 0.0399(5) Uani 1 1 d . . . . .
N5 N 0.6701(2) 0.30979(19) 0.41482(12) 0.0462(6) Uani 1 1 d . . . . .
H5A H 0.646009 0.281145 0.374750 0.055 Uiso 1 1 calc R . . . .
H5B H 0.612634 0.326496 0.439576 0.055 Uiso 1 1 calc R . . . .
N6 N 1.0875(2) 0.3063(2) 0.38510(13) 0.0520(6) Uani 1 1 d . . . . .
H6A H 1.065098 0.278808 0.344426 0.062 Uiso 1 1 calc R . . . .
H6B H 1.168172 0.321269 0.400367 0.062 Uiso 1 1 calc R . . . .
N7 N 0.6144(2) 0.41426(14) 0.67244(11) 0.0337(4) Uani 1 1 d . . . . .
N8 N 0.7138(2) 0.26750(16) 0.61934(11) 0.0381(5) Uani 1 1 d . . . . .
N9 N 0.5260(2) 0.31703(18) 0.75009(12) 0.0427(5) Uani 1 1 d . . . . .
N10 N 0.4913(2) 0.48130(18) 0.75144(12) 0.0434(5) Uani 1 1 d . . . . .
N11 N 0.5865(3) 0.57230(17) 0.67988(13) 0.0444(5) Uani 1 1 d . . . . .
H11A H 0.555351 0.621441 0.697752 0.053 Uiso 1 1 calc R . . . .
H11B H 0.633141 0.579081 0.647420 0.053 Uiso 1 1 calc R . . . .
N12 N 0.3986(3) 0.3839(2) 0.82003(14) 0.0576(7) Uani 1 1 d . . . . .
H12A H 0.362842 0.432653 0.835736 0.069 Uiso 1 1 calc R . . . .
H12B H 0.384834 0.328043 0.835387 0.069 Uiso 1 1 calc R . . . .
O1 O 0.53105(16) 0.38457(14) 0.51201(9) 0.0378(4) Uani 1 1 d . . . . .
O2 O 0.31687(16) 0.44924(13) 0.44799(9) 0.0370(4) Uani 1 1 d . . . . .
P1 P 0.39215(6) 0.40443(5) 0.51199(3) 0.03616(19) Uani 1 1 d . . . . .
H1A H 0.380(3) 0.450(2) 0.5641(16) 0.038(8) Uiso 1 1 d . . . . .
O3 O 0.3326(7) 0.3181(6) 0.5333(6) 0.128(4) Uani 0.5 1 d . . P . .
C3A C 0.3806(14) 0.2253(8) 0.5361(7) 0.115(4) Uani 0.5 1 d . . P . .
H3AA H 0.311731 0.182924 0.515535 0.173 Uiso 0.5 1 calc R . P . .
H3AB H 0.412463 0.207824 0.584647 0.173 Uiso 0.5 1 calc R . P . .
H3AC H 0.450701 0.221558 0.509840 0.173 Uiso 0.5 1 calc R . P . .
N1A N 0.8230(5) 0.3290(3) 0.8585(3) 0.0533(7) Uani 0.677(5) 1 d . U P A 1
O1A O 0.7553(4) 0.3798(3) 0.8877(2) 0.0688(11) Uani 0.677(5) 1 d . U P A 1
O2A O 0.8638(12) 0.2493(9) 0.8871(7) 0.093(3) Uani 0.677(5) 1 d . U P A 1
O3A O 0.8555(4) 0.3581(3) 0.8028(2) 0.0601(10) Uani 0.677(5) 1 d . U P A 1
N1B N 0.8760(9) 0.2962(6) 0.8402(5) 0.0533(7) Uani 0.323(5) 1 d . U P A 2
O1B O 0.7995(11) 0.3581(8) 0.8277(7) 0.075(2) Uani 0.323(5) 1 d . U P A 2
O2B O 0.8601(14) 0.2508(9) 0.8830(9) 0.045(2) Uani 0.323(5) 1 d . U P A 2
O3B O 0.9650(10) 0.2768(7) 0.8042(5) 0.079(3) Uani 0.323(5) 1 d . U P A 2
C1C C 1.0870(8) 0.2473(6) 0.7140(4) 0.0661(19) Uani 0.5 1 d . U P B -1
H1CA H 1.016038 0.239690 0.674464 0.099 Uiso 0.5 1 calc R . P B -1
H1CB H 1.151974 0.199545 0.711859 0.099 Uiso 0.5 1 calc R . P B -1
H1CC H 1.125221 0.308935 0.712006 0.099 Uiso 0.5 1 calc R . P B -1
O1C O 1.0409(3) 0.2381(2) 0.77638(17) 0.0347(7) Uani 0.5 1 d . U P B -1
H1C H 0.984320 0.278451 0.777890 0.052 Uiso 0.5 1 calc . . P C -1
C1D C 1.2134(14) 0.1791(10) 0.6411(7) 0.0588(18) Uani 0.25 1 d . U P D -2
H1DA H 1.131191 0.177975 0.608592 0.088 Uiso 0.25 1 calc R . P D -2
H1DB H 1.258266 0.120113 0.638248 0.088 Uiso 0.25 1 calc R . P D -2
H1DC H 1.265920 0.230278 0.628855 0.088 Uiso 0.25 1 calc R . P D -2
O1D O 1.1930(9) 0.1911(7) 0.7053(5) 0.0588(18) Uani 0.25 1 d . U P D -2
H1D H 1.170263 0.140502 0.720635 0.088 Uiso 0.25 1 calc . . P E -2
O1E O 1.2211(11) 0.0107(8) 0.5924(6) 0.068(2) Uani 0.25 1 d D U P F -8
H1E H 1.199610 0.046873 0.558465 0.102 Uiso 0.25 1 calc . . P G -8
C1E C 1.3148(19) -0.0516(15) 0.5777(11) 0.079(5) Uani 0.25 1 d D U P F -8
H1EA H 1.275972 -0.094159 0.540569 0.119 Uiso 0.25 1 calc R . P F -8
H1EB H 1.349372 -0.087322 0.619694 0.119 Uiso 0.25 1 calc R . P F -8
H1EC H 1.384108 -0.016819 0.562657 0.119 Uiso 0.25 1 calc R . P F -8
C1F C 1.3157(14) 0.0403(10) 0.5732(6) 0.064(3) Uani 0.25 1 d D U P H -3
H1FA H 1.255061 0.022034 0.531211 0.097 Uiso 0.25 1 calc R . P H -3
H1FB H 1.373883 -0.011558 0.588655 0.097 Uiso 0.25 1 calc R . P H -3
H1FC H 1.365336 0.094113 0.562782 0.097 Uiso 0.25 1 calc R . P H -3
O1F O 1.2478(10) 0.0635(7) 0.6263(4) 0.056(2) Uani 0.25 1 d D U P H -3
H1F H 1.168940 0.064841 0.609791 0.084 Uiso 0.25 1 calc . . P I -3
O1G O 1.049(3) 0.109(2) 0.5270(16) 0.091(7) Uiso 0.125 1 d D . P J -4
H1G H 1.127202 0.114979 0.524690 0.137 Uiso 0.125 1 calc . . P K -4
C1G C 1.003(6) 0.025(2) 0.496(3) 0.100(13) Uiso 0.125 1 d D . P J -4
H1GA H 1.035115 -0.026081 0.527500 0.150 Uiso 0.125 1 calc R . P J -4
H1GB H 1.031532 0.017683 0.451881 0.150 Uiso 0.125 1 calc R . P J -4
H1GC H 0.908859 0.025763 0.488293 0.150 Uiso 0.125 1 calc R . P J -4
O1H O 1.346(2) -0.0741(14) 0.5838(10) 0.044(4) Uiso 0.125 1 d D . P L -5
H1H H 1.371135 -0.060927 0.626034 0.066 Uiso 0.125 1 calc . . P M -5
C1H C 1.4277(19) -0.0332(15) 0.5442(11) 0.040(4) Uiso 0.125 1 d D . P L -5
H1HA H 1.398334 0.030005 0.531360 0.060 Uiso 0.125 1 calc R . P L -5
H1HB H 1.427174 -0.069980 0.501960 0.060 Uiso 0.125 1 calc R . P L -5
H1HC H 1.514890 -0.031051 0.571544 0.060 Uiso 0.125 1 calc R . P L -5
O1J O 1.3922(18) -0.0534(13) 0.5781(9) 0.045(3) Uiso 0.125 1 d D U P N -6
H1J H 1.443261 -0.035539 0.552749 0.068 Uiso 0.125 1 calc . . P O -6
C1J C 1.270(2) -0.018(3) 0.5520(19) 0.072(5) Uiso 0.125 1 d D U P N -6
H1JA H 1.244732 0.025099 0.585758 0.108 Uiso 0.125 1 calc R . P N -6
H1JB H 1.208135 -0.069692 0.544015 0.108 Uiso 0.125 1 calc R . P N -6
H1JC H 1.270382 0.014135 0.508007 0.108 Uiso 0.125 1 calc R . P N -6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 -0.2673 2.5549 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 '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
C2 C1 H1 118.6 . .
N1 C1 H1 118.6 . .
N1 C1 C2 122.8(3) . .
C1 C2 H2 120.5 . .
C3 C2 C1 118.9(3) . .
C3 C2 H2 120.5 . .
C2 C3 H3 120.7 . .
C2 C3 C4 118.7(3) . .
C4 C3 H3 120.7 . .
C3 C4 H4 120.5 . .
C5 C4 C3 119.0(2) . .
C5 C4 H4 120.5 . .
C4 C5 C6 121.3(2) . .
N1 C5 C4 122.2(2) . .
N1 C5 C6 116.6(2) . .
N2 C6 C5 116.3(2) . .
N4 C6 C5 116.4(2) . .
N4 C6 N2 127.3(2) . .
N3 C7 N2 124.2(2) . .
N5 C7 N2 117.3(2) . .
N5 C7 N3 118.4(2) . .
N3 C8 N4 125.1(2) . .
N6 C8 N3 118.3(2) . .
N6 C8 N4 116.6(2) . .
C10 C9 H9 118.4 . .
N8 C9 H9 118.4 . .
N8 C9 C10 123.2(3) . .
C9 C10 H10 120.6 . .
C11 C10 C9 118.8(3) . .
C11 C10 H10 120.6 . .
C10 C11 H11 120.6 . .
C10 C11 C12 118.8(3) . .
C12 C11 H11 120.6 . .
C11 C12 H12 120.2 . .
C13 C12 C11 119.5(3) . .
C13 C12 H12 120.2 . .
C12 C13 C14 122.1(2) . .
N8 C13 C12 121.9(2) . .
N8 C13 C14 116.0(2) . .
N7 C14 C13 115.8(2) . .
N9 C14 C13 117.4(2) . .
N9 C14 N7 126.8(2) . .
N10 C15 N9 125.3(2) . .
N10 C15 N12 117.2(3) . .
N12 C15 N9 117.5(3) . .
N10 C16 N7 124.4(2) . .
N11 C16 N7 117.6(2) . .
N11 C16 N10 118.0(2) . .
N1 Fe1 N2 75.49(8) . .
N1 Fe1 N7 98.07(8) . .
N1 Fe1 N8 92.61(9) . .
N2 Fe1 N7 164.12(8) . .
N8 Fe1 N2 91.64(8) . .
N8 Fe1 N7 73.96(8) . .
O1 Fe1 N1 169.17(8) . .
O1 Fe1 N2 94.60(7) . .
O1 Fe1 N7 92.62(7) . .
O1 Fe1 N8 92.02(8) . .
O1 Fe1 O2 87.94(8) . 3_666
O2 Fe1 N1 88.96(8) 3_666 .
O2 Fe1 N2 97.05(7) 3_666 .
O2 Fe1 N7 97.33(7) 3_666 .
O2 Fe1 N8 171.29(7) 3_666 .
C1 N1 C5 118.5(2) . .
C1 N1 Fe1 125.02(17) . .
C5 N1 Fe1 116.28(17) . .
C6 N2 C7 113.9(2) . .
C6 N2 Fe1 114.92(16) . .
C7 N2 Fe1 130.93(16) . .
C8 N3 C7 115.3(2) . .
C6 N4 C8 114.1(2) . .
C7 N5 H5A 120.0 . .
C7 N5 H5B 120.0 . .
H5A N5 H5B 120.0 . .
C8 N6 H6A 120.0 . .
C8 N6 H6B 120.0 . .
H6A N6 H6B 120.0 . .
C14 N7 C16 114.0(2) . .
C14 N7 Fe1 116.18(16) . .
C16 N7 Fe1 129.38(17) . .
C9 N8 C13 117.8(2) . .
C9 N8 Fe1 124.82(18) . .
C13 N8 Fe1 117.19(17) . .
C14 N9 C15 114.2(2) . .
C15 N10 C16 115.2(2) . .
C16 N11 H11A 120.0 . .
C16 N11 H11B 120.0 . .
H11A N11 H11B 120.0 . .
C15 N12 H12A 120.0 . .
C15 N12 H12B 120.0 . .
H12A N12 H12B 120.0 . .
P1 O1 Fe1 136.46(11) . .
P1 O2 Fe1 129.96(11) . 3_666
O1 P1 H1A 110.7(14) . .
O2 P1 O1 116.98(10) . .
O2 P1 H1A 109.7(14) . .
O3 P1 O1 108.0(3) . .
O3 P1 O2 113.9(4) . .
O3 P1 H1A 95.6(15) . .
C3A O3 P1 128.6(7) . .
O3 C3A H3AA 109.5 . .
O3 C3A H3AB 109.5 . .
O3 C3A H3AC 109.5 . .
H3AA C3A H3AB 109.5 . .
H3AA C3A H3AC 109.5 . .
H3AB C3A H3AC 109.5 . .
O1A N1A O2A 119.6(7) . .
O1A N1A O3A 118.3(5) . .
O3A N1A O2A 122.0(6) . .
O1B N1B O3B 125.3(11) . .
O2B N1B O1B 113.8(12) . .
O2B N1B O3B 120.7(10) . .
H1CA C1C H1CB 109.5 . .
H1CA C1C H1CC 109.5 . .
H1CB C1C H1CC 109.5 . .
O1C C1C H1CA 109.5 . .
O1C C1C H1CB 109.5 . .
O1C C1C H1CC 109.5 . .
C1C O1C H1C 109.5 . .
H1DA C1D H1DB 109.5 . .
H1DA C1D H1DC 109.5 . .
H1DB C1D H1DC 109.5 . .
O1D C1D H1DA 109.5 . .
O1D C1D H1DB 109.5 . .
O1D C1D H1DC 109.5 . .
C1D O1D H1D 109.5 . .
C1E O1E H1E 109.5 . .
O1E C1E H1EA 109.5 . .
O1E C1E H1EB 109.5 . .
O1E C1E H1EC 109.5 . .
H1EA C1E H1EB 109.5 . .
H1EA C1E H1EC 109.5 . .
H1EB C1E H1EC 109.5 . .
H1FA C1F H1FB 109.5 . .
H1FA C1F H1FC 109.5 . .
H1FB C1F H1FC 109.5 . .
O1F C1F H1FA 109.5 . .
O1F C1F H1FB 109.5 . .
O1F C1F H1FC 109.5 . .
C1F O1F H1F 109.5 . .
C1G O1G H1G 109.5 . .
O1G C1G H1GA 109.5 . .
O1G C1G H1GB 109.5 . .
O1G C1G H1GC 109.5 . .
H1GA C1G H1GB 109.5 . .
H1GA C1G H1GC 109.5 . .
H1GB C1G H1GC 109.5 . .
C1H O1H H1H 109.5 . .
O1H C1H H1HA 109.5 . .
O1H C1H H1HB 109.5 . .
O1H C1H H1HC 109.5 . .
H1HA C1H H1HB 109.5 . .
H1HA C1H H1HC 109.5 . .
H1HB C1H H1HC 109.5 . .
C1J O1J H1J 109.5 . .
O1J C1J H1JA 109.5 . .
O1J C1J H1JB 109.5 . .
O1J C1J H1JC 109.5 . .
H1JA C1J H1JB 109.5 . .
H1JA C1J H1JC 109.5 . .
H1JB C1J H1JC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 H1 0.9500 .
C1 C2 1.384(4) .
C1 N1 1.337(3) .
C2 H2 0.9500 .
C2 C3 1.379(4) .
C3 H3 0.9500 .
C3 C4 1.390(4) .
C4 H4 0.9500 .
C4 C5 1.387(4) .
C5 C6 1.488(3) .
C5 N1 1.341(3) .
C6 N2 1.345(3) .
C6 N4 1.313(3) .
C7 N2 1.369(3) .
C7 N3 1.346(3) .
C7 N5 1.318(3) .
C8 N3 1.340(3) .
C8 N4 1.365(3) .
C8 N6 1.330(3) .
C9 H9 0.9500 .
C9 C10 1.385(4) .
C9 N8 1.342(4) .
C10 H10 0.9500 .
C10 C11 1.368(5) .
C11 H11 0.9500 .
C11 C12 1.385(5) .
C12 H12 0.9500 .
C12 C13 1.385(4) .
C13 C14 1.487(4) .
C13 N8 1.344(3) .
C14 N7 1.336(3) .
C14 N9 1.326(3) .
C15 N9 1.358(4) .
C15 N10 1.338(4) .
C15 N12 1.339(4) .
C16 N7 1.371(3) .
C16 N10 1.345(3) .
C16 N11 1.320(4) .
Fe1 N1 2.172(2) .
Fe1 N2 2.2165(19) .
Fe1 N7 2.228(2) .
Fe1 N8 2.190(2) .
Fe1 O1 2.0923(18) .
Fe1 O2 2.1010(18) 3_666
N5 H5A 0.8800 .
N5 H5B 0.8800 .
N6 H6A 0.8800 .
N6 H6B 0.8800 .
N11 H11A 0.8800 .
N11 H11B 0.8800 .
N12 H12A 0.8800 .
N12 H12B 0.8800 .
O1 P1 1.5026(18) .
O2 P1 1.4995(19) .
P1 H1A 1.24(3) .
P1 O3 1.488(7) .
O3 C3A 1.428(15) .
C3A H3AA 0.9800 .
C3A H3AB 0.9800 .
C3A H3AC 0.9800 .
N1A O1A 1.235(6) .
N1A O2A 1.314(14) .
N1A O3A 1.273(7) .
N1B O1B 1.199(15) .
N1B O2B 1.098(19) .
N1B O3B 1.310(14) .
C1C H1CA 0.9800 .
C1C H1CB 0.9800 .
C1C H1CC 0.9800 .
C1C O1C 1.402(7) .
O1C H1C 0.8400 .
C1D H1DA 0.9800 .
C1D H1DB 0.9800 .
C1D H1DC 0.9800 .
C1D O1D 1.324(16) .
O1D H1D 0.8400 .
O1E H1E 0.8400 .
O1E C1E 1.408(5) .
C1E H1EA 0.9800 .
C1E H1EB 0.9800 .
C1E H1EC 0.9800 .
C1F H1FA 0.9800 .
C1F H1FB 0.9800 .
C1F H1FC 0.9800 .
C1F O1F 1.409(5) .
O1F H1F 0.8400 .
O1G H1G 0.8400 .
O1G C1G 1.399(5) .
C1G H1GA 0.9800 .
C1G H1GB 0.9800 .
C1G H1GC 0.9800 .
O1H H1H 0.8400 .
O1H C1H 1.394(5) .
C1H H1HA 0.9800 .
C1H H1HB 0.9800 .
C1H H1HC 0.9800 .
O1J H1J 0.8400 .
O1J C1J 1.400(5) .
C1J H1JA 0.9800 .
C1J H1JB 0.9800 .
C1J H1JC 0.9800 .
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
_geom_hbond_publ_flag
N5 H5A O3B 0.88 2.30 3.038(9) 140.8 4_565 yes
N5 H5A O1C 0.88 2.05 2.881(4) 156.0 4_565 yes
N5 H5B O1 0.88 1.98 2.826(3) 161.8 . yes
N6 H6A N9 0.88 2.28 3.146(3) 168.8 4_665 yes
N6 H6B O2 0.88 2.49 3.251(3) 144.9 1_655 yes
N6 H6B O2A 0.88 2.37 3.034(12) 132.5 4_665 yes
N6 H6B O2B 0.88 2.37 3.017(12) 130.8 4_665 yes
N11 H11A O3B 0.88 2.25 3.021(9) 146.7 2_656 yes
N11 H11A O1C 0.88 2.08 2.948(4) 170.0 2_656 yes
N11 H11B O2 0.88 2.07 2.889(3) 154.1 3_666 yes
N11 H11B O2B 0.88 2.55 2.949(12) 108.6 2_656 yes
N12 H12A O1F 0.88 2.41 3.288(11) 176.3 2_656 yes
N12 H12B N3 0.88 2.24 3.103(4) 166.1 4_566 yes
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
C1 C2 C3 C4 -1.0(5) . . . .
C2 C1 N1 C5 0.6(5) . . . .
C2 C1 N1 Fe1 -173.4(3) . . . .
C2 C3 C4 C5 0.7(5) . . . .
C3 C4 C5 C6 -178.5(3) . . . .
C3 C4 C5 N1 0.3(4) . . . .
C4 C5 C6 N2 -175.2(2) . . . .
C4 C5 C6 N4 5.7(4) . . . .
C4 C5 N1 C1 -0.9(4) . . . .
C4 C5 N1 Fe1 173.6(2) . . . .
C5 C6 N2 C7 -176.2(2) . . . .
C5 C6 N2 Fe1 -1.4(3) . . . .
C5 C6 N4 C8 176.9(2) . . . .
C6 C5 N1 C1 177.9(3) . . . .
C6 C5 N1 Fe1 -7.5(3) . . . .
C9 C10 C11 C12 -0.2(6) . . . .
C10 C9 N8 C13 1.1(5) . . . .
C10 C9 N8 Fe1 -173.7(3) . . . .
C10 C11 C12 C13 0.3(6) . . . .
C11 C12 C13 C14 179.7(3) . . . .
C11 C12 C13 N8 0.4(5) . . . .
C12 C13 C14 N7 178.1(3) . . . .
C12 C13 C14 N9 -2.4(4) . . . .
C12 C13 N8 C9 -1.1(4) . . . .
C12 C13 N8 Fe1 174.1(2) . . . .
C13 C14 N7 C16 -177.9(2) . . . .
C13 C14 N7 Fe1 8.8(3) . . . .
C13 C14 N9 C15 -178.8(2) . . . .
C14 C13 N8 C9 179.5(3) . . . .
C14 C13 N8 Fe1 -5.3(3) . . . .
Fe1 O1 P1 O2 129.56(16) . . . .
Fe1 O1 P1 O3 -100.5(5) . . . .
Fe1 O2 P1 O1 -86.67(16) 3_666 . . .
Fe1 O2 P1 O3 146.1(4) 3_666 . . .
N1 C1 C2 C3 0.3(5) . . . .
N1 C5 C6 N2 5.9(3) . . . .
N1 C5 C6 N4 -173.1(2) . . . .
N2 C6 N4 C8 -2.1(4) . . . .
N2 C7 N3 C8 -3.6(4) . . . .
N3 C7 N2 C6 0.3(4) . . . .
N3 C7 N2 Fe1 -173.47(19) . . . .
N3 C8 N4 C6 -1.8(4) . . . .
N4 C6 N2 C7 2.8(4) . . . .
N4 C6 N2 Fe1 177.6(2) . . . .
N4 C8 N3 C7 4.4(4) . . . .
N5 C7 N2 C6 179.5(2) . . . .
N5 C7 N2 Fe1 5.7(4) . . . .
N5 C7 N3 C8 177.3(3) . . . .
N6 C8 N3 C7 -175.7(3) . . . .
N6 C8 N4 C6 178.3(3) . . . .
N7 C14 N9 C15 0.6(4) . . . .
N7 C16 N10 C15 1.4(4) . . . .
N8 C9 C10 C11 -0.5(6) . . . .
N8 C13 C14 N7 -2.5(3) . . . .
N8 C13 C14 N9 177.0(2) . . . .
N9 C14 N7 C16 2.7(4) . . . .
N9 C14 N7 Fe1 -170.6(2) . . . .
N9 C15 N10 C16 2.4(4) . . . .
N10 C15 N9 C14 -3.3(4) . . . .
N10 C16 N7 C14 -3.7(4) . . . .
N10 C16 N7 Fe1 168.43(19) . . . .
N11 C16 N7 C14 175.9(2) . . . .
N11 C16 N7 Fe1 -11.9(4) . . . .
N11 C16 N10 C15 -178.2(3) . . . .
N12 C15 N9 C14 176.2(3) . . . .
N12 C15 N10 C16 -177.2(3) . . . .
O1 P1 O3 C3A -15.8(13) . . . .
O2 P1 O3 C3A 115.9(11) . . . .
