# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Fe2(bdp)3
_database_code_depnum_ccdc_archive 'CCDC 2010318'
loop_
_audit_author_name
_audit_author_address
'Naomi Biggins'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-06-17 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_audit_creation_date             2019-09-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Fe2(bdp)3(DMF)0.58
_chemical_name_systematic        Fe2(bdp)3
_chemical_formula_moiety         
'0.13(C288 H192 Fe16 N96), 4(C0.86 H2 N0.29 O0.29)'
_chemical_formula_sum            'C39.44 H32.02 Fe2 N13.14 O1.15'
_chemical_formula_weight         820.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0056 0.0027
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Fe Fe 0.3411 1.2586
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
N N 0.0104 0.0054
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
O O 0.0176 0.0099
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   7.0648(4)
_cell_length_b                   26.4382(14)
_cell_length_c                   45.215(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8445.3(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5036
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.74
_cell_measurement_theta_min      3.76
_shelx_estimated_absorpt_T_max   0.982
_shelx_estimated_absorpt_T_min   0.929
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1389 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.8053.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3374
_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 100 K by an Oxford Cryosystems Cyrostream using N2 during
 the experiments. Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.8856 angstrom) on a Bruker D8 diffractometer
equipped with a Bruker PHOTON II detector.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            22769
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.981
_diffrn_reflns_theta_max         30.981
_diffrn_reflns_theta_min         2.224
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1428
_reflns_number_total             1749
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_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)'
_refine_diff_density_max         2.622
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1749
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0718
_refine_ls_restrained_S_all      1.114
_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)+(0.1139P)²+128.2064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2123
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.

Disorder of the dimethylformamide solvent required displacement parameter restraints 
(RIGU and SIMU), distance restraints (DFIX) and geometric constraints (FLAT) in order to 
obtain a stable refinement. Without these restraints and constraints, anisotropic 
refiment resulted in several atoms with very enlarged or elongated thermal ellipsoids.
The site occupancy of the dimethylformamide solvent was allowed to refine freely, 
giving a value of 29%. 
Additionally, disorder of the benzene rings of the ligand required displacement 
parameter restraints (RIGU and SIMU).
;
_vrf_PLAT094_Fe2bdp3             
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.54 Report
RESPONSE: The residual electron density in question is located between the Fe 
atoms of the one-dimensional pyrazolate-bridged Fe chains, with a distance 
of 1.77594(13)A. Since this Q-peak is close to the heavy Fe atoms, it can 
likely be attributed to Fourier truncation errors.
;
_vrf_PLAT097_Fe2bdp3             
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.62 eA-3  
RESPONSE: The residual electron density in question is located between the Fe 
atoms of the one-dimensional pyrazolate-bridged Fe chains, with a distance 
of 1.77594(13)A. Since this Q-peak is close to the heavy Fe atoms, it can 
likely be attributed to Fourier truncation errors.
;
_vrf_PLAT971_Fe2bdp3             
;
PROBLEM: Check Calcd Resid. Dens.  1.68A   From N3              3.15 eA-3  
RESPONSE: The residual electron density in question is located between the Fe 
atoms of the one-dimensional pyrazolate-bridged Fe chains, with a distance 
of 1.77594(13)A. Since this Q-peak is close to the heavy Fe atoms, it can 
likely be attributed to Fourier truncation errors.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N4-C14
 1.327 with sigma of 0.06
 C14-O1
 1.231 with sigma of 0.06
 N4-C15
 1.44 with sigma of 0.05
 C16-N4
 1.441 with sigma of 0.05
 C15-C14
 2.41 with sigma of 0.08
 C16-C14
 2.41 with sigma of 0.08
3. Restrained planarity
 C15, N4, C16, C14
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C5 \\sim C4 \\sim C13 \\sim C11 \\sim C10 \\sim C12: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
O1 \\sim C14 \\sim N4 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C5, C4, C11, C10, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, N4, C16, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H16C)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(H16B)=Sof(H16A)=Sof(H15F)=
 Sof(H15A)=Sof(H15C)=Sof(H15B)=Sof(H15E)=Sof(H15D)=0.5*FVAR(2)
 Sof(C16)=Sof(N4)=Sof(C14)=Sof(H14)=Sof(O1)=Sof(C15)=FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=1-FVAR(2)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=FVAR(2)
 Fixed Sof: C5(0.5) H5(0.5) C4(0.5) H4(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C1(H1), C12(H12), C5(H5), C11(H11), C13(H13), C10(H10),
 C4(H4), C14(H14)
7.b Disordered Me refined with riding coordinates:
 C16(H16C,H16D,H16E,H16F,H16B,H16A), C15(H15F,H15A,H15C,H15B,H15E,H15D)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.375000 0.375000 0.62147(2) 0.0132(4) Uani 1 2 d S T P . .
N1 N 0.5318(6) 0.43549(15) 0.62156(9) 0.0161(9) Uani 1 1 d . . . . .
N2 N 0.2108(6) 0.40460(15) 0.59175(9) 0.0176(10) Uani 1 1 d . . . . .
N3 N 0.0211(6) 0.40650(15) 0.59701(9) 0.0161(9) Uani 1 1 d . . . . .
C7 C -0.0575(8) 0.4316(2) 0.57425(11) 0.0226(12) Uani 1 1 d . . . . .
H7 H -0.189014 0.438372 0.572377 0.027 Uiso 1 1 calc R . . . .
C6 C 0.2459(7) 0.4273(2) 0.56624(11) 0.0223(12) Uani 1 1 d . . . . .
H6 H 0.367700 0.430222 0.557504 0.027 Uiso 1 1 calc R . . . .
C1 C 0.4751(8) 0.48368(19) 0.61959(12) 0.0225(12) Uani 1 1 d . . . . .
H1 H 0.349725 0.494183 0.615124 0.027 Uiso 1 1 calc R . . . .
C8 C 0.0783(8) 0.4463(2) 0.55391(12) 0.0240(12) Uani 1 1 d . . . . .
C2 C 0.625000 0.5160(3) 0.625000 0.0251(18) Uani 1 2 d S T P . .
C9 C 0.0415(8) 0.4735(2) 0.52633(12) 0.0278(13) Uani 1 1 d . . . . .
C3 C 0.625000 0.5717(3) 0.625000 0.0302(19) Uani 1 2 d S T P . .
C12 C -0.132(3) 0.4697(12) 0.5123(5) 0.037(6) Uani 0.31(2) 1 d . U . A 1
H12 H -0.223116 0.446813 0.520138 0.044 Uiso 0.31(2) 1 calc R . . A 1
C5 C 0.463(3) 0.6524(7) 0.6174(4) 0.036(4) Uani 0.5 1 d . U . B -1
H5 H 0.351152 0.670307 0.612506 0.043 Uiso 0.5 1 calc R . . B -1
C11 C -0.1653(15) 0.5270(5) 0.4970(2) 0.038(3) Uani 0.69(2) 1 d . U . A 2
H11 H -0.280648 0.545199 0.495332 0.045 Uiso 0.69(2) 1 calc R . . A 2
C13 C -0.182(3) 0.4977(12) 0.4871(5) 0.034(6) Uani 0.31(2) 1 d . U . A 1
H13 H -0.307442 0.496989 0.479471 0.041 Uiso 0.31(2) 1 calc R . . A 1
C10 C -0.1248(14) 0.5011(5) 0.5230(2) 0.038(3) Uani 0.69(2) 1 d . U . A 2
H10 H -0.212683 0.502390 0.538914 0.045 Uiso 0.69(2) 1 calc R . . A 2
C4 C 0.466(3) 0.5987(7) 0.6169(4) 0.041(5) Uani 0.5 1 d . U . B -1
H4 H 0.355500 0.580906 0.610772 0.050 Uiso 0.5 1 calc R . . B -1
C16 C -0.123(9) 0.3637(18) 0.4523(10) 0.15(2) Uani 0.286(14) 1 d D U . C -1
H16C H -0.069850 0.369513 0.432554 0.174 Uiso 0.143(7) 1 calc R . . C -1
H16D H -0.197546 0.332473 0.452190 0.174 Uiso 0.143(7) 1 calc R . . C -1
H16E H -0.203917 0.392213 0.457808 0.174 Uiso 0.143(7) 1 calc R . . C -1
H16F H -0.244359 0.359953 0.462480 0.174 Uiso 0.143(7) 1 calc R . . C -1
H16B H -0.116663 0.396993 0.442844 0.174 Uiso 0.143(7) 1 calc R . . C -1
H16A H -0.110292 0.337253 0.437227 0.174 Uiso 0.143(7) 1 calc R . . C -1
N4 N 0.023(6) 0.3592(11) 0.4725(8) 0.116(12) Uani 0.286(14) 1 d D U . C -1
C14 C 0.050(6) 0.3521(14) 0.4993(8) 0.094(11) Uani 0.286(14) 1 d D U . C -1
H14 H -0.054728 0.362390 0.511063 0.112 Uiso 0.286(14) 1 calc R . . C -1
O1 O 0.180(4) 0.3348(13) 0.5144(7) 0.119(12) Uani 0.286(14) 1 d D U . C -1
C15 C 0.194(9) 0.369(3) 0.4561(12) 0.20(3) Uani 0.286(14) 1 d D U . C -1
H15F H 0.163267 0.374492 0.435248 0.241 Uiso 0.143(7) 1 calc R . . C -1
H15A H 0.255471 0.399563 0.464063 0.241 Uiso 0.143(7) 1 calc R . . C -1
H15C H 0.280138 0.340282 0.458033 0.241 Uiso 0.143(7) 1 calc R . . C -1
H15B H 0.302650 0.368399 0.469647 0.241 Uiso 0.143(7) 1 calc R . . C -1
H15E H 0.210447 0.343328 0.440833 0.241 Uiso 0.143(7) 1 calc R . . C -1
H15D H 0.185779 0.402609 0.446863 0.241 Uiso 0.143(7) 1 calc R . . C -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 N1 1.946(4) 2 ?
Fe01 N1 1.945(4) . ?
Fe01 N2 1.940(4) . ?
Fe01 N2 1.940(4) 2 ?
Fe01 N3 1.947(4) 12 ?
Fe01 N3 1.947(4) 11_455 ?
N1 N1 1.353(9) 11 ?
N1 C1 1.339(7) . ?
N2 N3 1.362(6) . ?
N2 C6 1.323(7) . ?
N3 C7 1.344(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(8) . ?
C6 H6 0.9500 . ?
C6 C8 1.402(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.382(7) . ?
C8 C9 1.463(8) . ?
C2 C3 1.475(11) . ?
C9 C12 1.39(2) . ?
C9 C11 1.370(12) 17_566 ?
C9 C13 1.39(2) 17_566 ?
C9 C10 1.392(11) . ?
C3 C5 1.374(19) 14 ?
C3 C4 1.38(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.40(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.421(15) . ?
C11 H11 0.9500 . ?
C11 C10 1.391(13) . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C4 H4 0.9500 . ?
C16 H16C 0.9800 . ?
C16 H16D 0.9800 . ?
C16 H16E 0.9800 . ?
C16 H16F 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 N4 1.38(4) . ?
N4 C14 1.24(4) . ?
N4 C15 1.44(4) . ?
C14 H14 0.9500 . ?
C14 O1 1.23(3) . ?
C15 H15F 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15E 0.9800 . ?
C15 H15D 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe01 N1 179.8(2) . 2 ?
N1 Fe01 N3 87.07(17) 2 12 ?
N1 Fe01 N3 92.77(17) . 12 ?
N1 Fe01 N3 87.07(17) . 11_455 ?
N1 Fe01 N3 92.77(17) 2 11_455 ?
N2 Fe01 N1 89.56(17) . 2 ?
N2 Fe01 N1 89.56(17) 2 . ?
N2 Fe01 N1 90.59(17) . . ?
N2 Fe01 N1 90.59(17) 2 2 ?
N2 Fe01 N2 92.3(2) 2 . ?
N2 Fe01 N3 91.01(17) . 11_455 ?
N2 Fe01 N3 175.29(17) . 12 ?
N2 Fe01 N3 91.00(17) 2 12 ?
N2 Fe01 N3 175.29(17) 2 11_455 ?
N3 Fe01 N3 85.9(2) 12 11_455 ?
N1 N1 Fe01 123.69(14) 11 . ?
C1 N1 Fe01 127.7(4) . . ?
C1 N1 N1 107.9(3) . 11 ?
N3 N2 Fe01 118.8(3) . . ?
C6 N2 Fe01 132.4(4) . . ?
C6 N2 N3 108.7(4) . . ?
N2 N3 Fe01 129.3(3) . 11_455 ?
C7 N3 Fe01 123.5(4) . 11_455 ?
C7 N3 N2 106.9(4) . . ?
N3 C7 H7 124.4 . . ?
N3 C7 C8 111.1(5) . . ?
C8 C7 H7 124.4 . . ?
N2 C6 H6 124.7 . . ?
N2 C6 C8 110.5(5) . . ?
C8 C6 H6 124.7 . . ?
N1 C1 H1 124.9 . . ?
N1 C1 C2 110.3(5) . . ?
C2 C1 H1 124.9 . . ?
C7 C8 C6 102.7(5) . . ?
C7 C8 C9 125.5(5) . . ?
C6 C8 C9 131.7(5) . . ?
C1 C2 C1 103.7(7) 11 . ?
C1 C2 C3 128.1(3) . . ?
C1 C2 C3 128.1(3) 11 . ?
C12 C9 C8 120.8(10) . . ?
C12 C9 C13 118.2(13) . 17_566 ?
C11 C9 C8 122.6(6) 17_566 . ?
C11 C9 C13 38.1(11) 17_566 17_566 ?
C11 C9 C10 117.5(7) 17_566 . ?
C13 C9 C8 121.0(10) 17_566 . ?
C10 C9 C8 120.0(6) . . ?
C10 C9 C13 105.6(12) . 17_566 ?
C5 C3 C2 119.8(8) 14 . ?
C5 C3 C4 110.7(9) 14 . ?
C4 C3 C2 121.0(9) . . ?
C9 C12 H12 118.1 . . ?
C9 C12 C13 123.7(18) . . ?
C13 C12 H12 118.1 . . ?
C3 C5 H5 120.2 8 . ?
C3 C5 C4 119.5(19) 8 . ?
C4 C5 H5 120.2 . . ?
C9 C11 H11 119.5 17_566 . ?
C9 C11 C10 121.1(9) 17_566 . ?
C10 C11 H11 119.5 . . ?
C9 C13 C12 117.7(18) 17_566 . ?
C9 C13 H13 121.2 17_566 . ?
C12 C13 H13 121.2 . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.5(8) . . ?
C11 C10 H10 119.3 . . ?
C3 C4 C5 121(2) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
H16C C16 H16D 109.5 . . ?
H16C C16 H16E 109.5 . . ?
H16D C16 H16E 109.5 . . ?
H16F C16 H16B 109.5 . . ?
H16F C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
N4 C16 H16C 109.5 . . ?
N4 C16 H16D 109.5 . . ?
N4 C16 H16E 109.5 . . ?
N4 C16 H16F 109.5 . . ?
N4 C16 H16B 109.5 . . ?
N4 C16 H16A 109.5 . . ?
C16 N4 C15 106(4) . . ?
C14 N4 C16 141(5) . . ?
C14 N4 C15 113(4) . . ?
N4 C14 H14 112.3 . . ?
O1 C14 N4 135(4) . . ?
O1 C14 H14 112.3 . . ?
N4 C15 H15F 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15F C15 H15A 109.5 . . ?
H15F C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15E 109.5 . . ?
H15B C15 H15D 109.5 . . ?
H15E C15 H15D 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Na05Fe2(bdp)3
_database_code_depnum_ccdc_archive 'CCDC 2010321'
loop_
_audit_author_name
_audit_author_address
'Naomi Biggins'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-06-17 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_audit_creation_date             2019-09-16
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Na0.5Fe2(bdp)3
_chemical_name_systematic        Na0.5Fe2(bdp)3
_chemical_formula_moiety         '0.13(C288 H192 Fe16 N96), 0.49(Na)'
_chemical_formula_sum            'C36 H24 Fe2 N12 Na0.51'
_chemical_formula_weight         748.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Fe Fe 0.3511 0.8892
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
N N 0.0065 0.0035
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Na Na 0.0389 0.0265
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   7.0813(16)
_cell_length_b                   26.493(7)
_cell_length_c                   45.483(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8533(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.41
_cell_measurement_theta_min      3.36
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.938
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1347 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.9327.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3053
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.021
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 100 K by an Oxford Cryosystems Cyrostream using N2 during
 the experiments. Data was collected at Beamline 12.2.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7288 angstrom) on a Bruker D8 diffractometer
equipped with a Bruker PHOTON II detector.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            42581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         31.310
_diffrn_reflns_theta_min         3.088
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2651
_reflns_number_total             3241
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_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)'
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3241
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0542
_refine_ls_restrained_S_all      1.094
_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)+(0.0945P)²+45.8228P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1677
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.

Disorder of the benzene rings of the ligand necessitated the use of displacement parameter restraints 
(SIMU and DELU).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C9, C10, C11, C13, C12
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 C4, C5
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9 \\sim C10 \\sim C11 \\sim C13 \\sim C12: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=1-FVAR(1)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=FVAR(1)
 Fixed Sof: C5(0.5) H5(0.5) C4(0.5) H4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C1(H1), C13(H13), C11(H11), C10(H10), C12(H12), C5(H5), C4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   diffmap
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 0.875000 0.375000 0.62140(2) 0.00703(15) Uani 1 2 d S T P . .
N2 N 0.7105(3) 0.40486(7) 0.59192(4) 0.0111(4) Uani 1 1 d . . . . .
N1 N 1.0314(3) 0.43544(7) 0.62165(4) 0.0109(4) Uani 1 1 d . . . . .
N3 N 0.5209(3) 0.40680(7) 0.59678(4) 0.0109(4) Uani 1 1 d . . . . .
C6 C 0.7466(3) 0.42804(9) 0.56626(5) 0.0163(5) Uani 1 1 d . . . . .
H6 H 0.868313 0.431841 0.557768 0.020 Uiso 1 1 calc R . . . .
C7 C 0.4413(4) 0.43097(9) 0.57413(5) 0.0157(4) Uani 1 1 d . . . . .
H7 H 0.309791 0.437139 0.572168 0.019 Uiso 1 1 calc R . . . .
C8 C 0.5773(4) 0.44584(10) 0.55384(5) 0.0180(5) Uani 1 1 d . . . . .
C2 C 1.125000 0.51628(12) 0.625000 0.0166(6) Uani 1 2 d S T P . .
C1 C 0.9746(4) 0.48367(9) 0.61953(5) 0.0160(5) Uani 1 1 d . . . . .
H1 H 0.849657 0.494085 0.614951 0.019 Uiso 1 1 calc R . . . .
C3 C 1.125000 0.57151(13) 0.625000 0.0210(7) Uani 1 2 d S T P . .
C9 C 0.5406(4) 0.47320(11) 0.52633(5) 0.0221(5) Uani 1 1 d . U . . .
C13 C 0.6363(9) 0.5294(4) 0.48696(18) 0.028(2) Uani 0.513(19) 1 d . U . A 1
H13 H 0.731842 0.549585 0.478206 0.033 Uiso 0.513(19) 1 calc R . . A 1
C11 C 0.3266(13) 0.5229(6) 0.4956(2) 0.042(3) Uani 0.487(19) 1 d . U . A 2
H11 H 0.205123 0.537353 0.492873 0.051 Uiso 0.487(19) 1 calc R . . A 2
C10 C 0.3680(13) 0.4977(6) 0.5222(2) 0.044(3) Uani 0.487(19) 1 d . U . A 2
H10 H 0.276959 0.497452 0.537505 0.053 Uiso 0.487(19) 1 calc R . . A 2
C12 C 0.6769(10) 0.5031(4) 0.51282(18) 0.0266(19) Uani 0.513(19) 1 d . U . A 1
H12 H 0.799109 0.505656 0.521290 0.032 Uiso 0.513(19) 1 calc R . . A 1
Na2 Na -0.375000 0.625000 0.4984(4) 0.042(6) Uani 0.133(9) 2 d S T P B 1
C5 C 0.9638(17) 0.6516(4) 0.6186(2) 0.033(2) Uani 0.5 1 d . U . C -1
H5 H 0.850524 0.669285 0.614297 0.040 Uiso 0.5 1 calc R . . C -1
C4 C 0.9626(18) 0.5985(5) 0.6183(2) 0.036(3) Uani 0.5 1 d . U . C -1
H4 H 0.849658 0.580992 0.613565 0.043 Uiso 0.5 1 calc R . . C -1
Na1 Na -0.375000 0.625000 0.5505(17) 0.16(3) Uani 0.113(15) 2 d S T P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 N2 1.9445(19) . ?
Fe01 N2 1.9445(19) 2_655 ?
Fe01 N1 1.9469(19) 2_655 ?
Fe01 N1 1.9469(19) . ?
Fe01 N3 1.9677(18) 11 ?
Fe01 N3 1.9677(18) 12 ?
N2 N3 1.362(3) . ?
N2 C6 1.343(3) . ?
N1 N1 1.360(4) 11_655 ?
N1 C1 1.343(3) . ?
N3 C7 1.337(3) . ?
C6 H6 0.9500 . ?
C6 C8 1.406(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.391(3) . ?
C8 C9 1.469(3) . ?
C2 C1 1.394(3) . ?
C2 C1 1.394(3) 11_655 ?
C2 C3 1.463(5) . ?
C1 H1 0.9500 . ?
C3 C5 1.377(12) 8 ?
C3 C4 1.388(12) . ?
C9 C13 1.392(6) 17_666 ?
C9 C11 1.376(8) 17_666 ?
C9 C10 1.397(8) . ?
C9 C12 1.391(7) . ?
C9 Na2 3.067(8) 17_566 ?
C13 H13 0.9500 . ?
C13 C12 1.397(8) . ?
C13 Na2 2.587(12) 1_655 ?
C11 H11 0.9500 . ?
C11 C10 1.410(10) . ?
C10 H10 0.9500 . ?
C12 H12 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.405(7) . ?
C4 H4 0.9500 . ?

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
N2 Fe01 N2 92.79(11) . 2_655 ?
N2 Fe01 N1 89.88(8) 2_655 . ?
N2 Fe01 N1 90.59(8) 2_655 2_655 ?
N2 Fe01 N1 90.59(8) . . ?
N2 Fe01 N1 89.88(8) . 2_655 ?
N2 Fe01 N3 91.07(8) 2_655 12 ?
N2 Fe01 N3 174.86(8) 2_655 11 ?
N2 Fe01 N3 91.07(8) . 11 ?
N2 Fe01 N3 174.86(8) . 12 ?
N1 Fe01 N1 179.32(11) . 2_655 ?
N1 Fe01 N3 92.81(8) . 12 ?
N1 Fe01 N3 92.81(8) 2_655 11 ?
N1 Fe01 N3 86.69(8) . 11 ?
N1 Fe01 N3 86.69(8) 2_655 12 ?
N3 Fe01 N3 85.29(11) 12 11 ?
N3 N2 Fe01 119.61(13) . . ?
C6 N2 Fe01 132.17(16) . . ?
C6 N2 N3 108.14(18) . . ?
N1 N1 Fe01 123.76(6) 11_655 . ?
C1 N1 Fe01 127.71(17) . . ?
C1 N1 N1 107.93(14) . 11_655 ?
N2 N3 Fe01 128.38(14) . 11 ?
C7 N3 Fe01 123.40(16) . 11 ?
C7 N3 N2 107.96(18) . . ?
N2 C6 H6 125.1 . . ?
N2 C6 C8 109.9(2) . . ?
C8 C6 H6 125.1 . . ?
N3 C7 H7 124.6 . . ?
N3 C7 C8 110.8(2) . . ?
C8 C7 H7 124.6 . . ?
C6 C8 C9 131.2(2) . . ?
C7 C8 C6 103.2(2) . . ?
C7 C8 C9 125.6(2) . . ?
C1 C2 C1 103.4(3) 11_655 . ?
C1 C2 C3 128.30(15) 11_655 . ?
C1 C2 C3 128.31(15) . . ?
N1 C1 C2 110.4(2) . . ?
N1 C1 H1 124.8 . . ?
C2 C1 H1 124.8 . . ?
C5 C3 C2 121.2(5) 8 . ?
C5 C3 C4 24.8(5) 8 . ?
C4 C3 C2 121.0(5) . . ?
C8 C9 Na2 87.8(3) . 17_566 ?
C13 C9 C8 120.3(3) 17_666 . ?
C13 C9 Na2 57.0(5) 17_666 17_566 ?
C11 C9 C8 122.3(4) 17_666 . ?
C11 C9 C10 117.7(4) 17_666 . ?
C11 C9 Na2 93.4(8) 17_666 17_566 ?
C10 C9 C8 120.0(4) . . ?
C10 C9 Na2 90.6(8) . 17_566 ?
C12 C9 C8 122.3(3) . . ?
C12 C9 C13 117.4(4) . 17_666 ?
C12 C9 Na2 125.9(6) . 17_566 ?
C9 C13 H13 119.1 17_666 . ?
C9 C13 C12 121.7(5) 17_666 . ?
C9 C13 Na2 96.2(6) 17_666 1_655 ?
C12 C13 H13 119.1 . . ?
C12 C13 Na2 109.0(7) . 1_655 ?
Na2 C13 H13 63.6 1_655 . ?
C9 C11 H11 119.5 17_666 . ?
C9 C11 C10 121.0(7) 17_666 . ?
C10 C11 H11 119.5 . . ?
C9 C10 H13 91.5(7) . 17_666 ?
C9 C10 C11 121.2(6) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C9 C12 C13 120.9(5) . . ?
C9 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
H13 Na2 H13 133.5 1_455 14_455 ?
C3 C5 H5 119.2 8 . ?
C3 C5 C4 121.7(12) 8 . ?
C4 C5 H5 119.2 . . ?
C3 C4 C5 120.6(13) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_K2Fe2(bdp)3
_database_code_depnum_ccdc_archive 'CCDC 2010319'
loop_
_audit_author_name
_audit_author_address
'Naomi Biggins'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-06-17 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_audit_creation_date             2019-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            K2Fe2(bdp)3
_chemical_name_systematic        K2Fe2(bdp)3
_chemical_formula_moiety         '0.13(C288 H192 Fe16 N96), 2.04(K)'
_chemical_formula_sum            'C36 H24 Fe2 K2.01 N12'
_chemical_formula_weight         815.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Fe Fe 0.3511 0.8892
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
K K 0.2084 0.2634
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
N N 0.0065 0.0035
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   7.081(3)
_cell_length_b                   26.535(9)
_cell_length_c                   45.388(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8528(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      3.36
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.973
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1547 before and 0.0738 after correction.
The Ratio of minimum to maximum transmission is 0.8305.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3314
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 100 K by an Oxford Cryosystems Cyrostream using N2 during
 the experiments. Data was collected at Beamline 11.3.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.8856 angstrom) on a Bruker D8 diffractometer
equipped with a Bruker PHOTON II detector.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            37407
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         28.995
_diffrn_reflns_theta_min         1.823
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2220
_reflns_number_total             2645
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_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)'
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2645
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0504
_refine_ls_restrained_S_all      1.146
_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)+(0.0715P)²+47.6197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1457
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.

Disorder of the potassium cations required displacement parameter restraints (SIMU and RIGU) to 
prevent anisotropic refinement from resulting in elongated and enlarged thermal ellipsoids.
A linear free variable restraint (SUMP) was used on the three-component potassium cation 
disorder to restrain the sum of the occupation factors to unity. In the absence of this 
restraint, the sum of the three-component disorder was greater than one.

Additionally, disorder of the benzene rings of the ligand required displacement parameter restraints 
(SIMU and DELU). 
;
_vrf_PLAT260_K2Fe2bdp3           
;
PROBLEM: Large Average Ueq of Residue Including        K1      0.314 Check 
RESPONSE: The potassium cations are highly disordered within the pores of the 
Fe2(bdp)3 framework. The large Ueq value likely arises from this disorder.
;

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
K3 \\sim K1 \\sim K2: within 3.5A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C10 \\sim C13 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 K3, K1, K2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(K1)]+1*[Sof(K3)]+1*[Sof(K2)]=1 with esd of 0.01
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=1-FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=FVAR(1)
 Fixed Sof: C4(0.5) H4(0.5) C5(0.5) H5(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C4(H4), C10(H10), C12(H12), C11(H11), C13(H13), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.125000 0.625000 0.37853(2) 0.01219(17) Uani 1 2 d S T P . .
N1 N 0.2815(3) 0.68545(8) 0.37839(4) 0.0168(4) Uani 1 1 d . . . . .
N2 N 0.2894(3) 0.59522(7) 0.40807(4) 0.0167(4) Uani 1 1 d . . . . .
N3 N 0.4786(3) 0.59326(8) 0.40324(4) 0.0164(4) Uani 1 1 d . . . . .
C1 C 0.2241(4) 0.73365(9) 0.38041(6) 0.0219(5) Uani 1 1 d . . . . .
H1 H 0.098949 0.744034 0.384867 0.026 Uiso 1 1 calc R . . . .
C2 C 0.375000 0.76625(14) 0.375000 0.0236(7) Uani 1 2 d S T P A .
C6 C 0.2540(4) 0.57194(10) 0.43380(5) 0.0225(5) Uani 1 1 d . . . . .
H6 H 0.132453 0.568114 0.442363 0.027 Uiso 1 1 calc R . . . .
C8 C 0.4224(4) 0.55418(11) 0.44610(6) 0.0244(6) Uani 1 1 d . . . . .
C7 C 0.5579(4) 0.56888(10) 0.42585(5) 0.0219(5) Uani 1 1 d . . . . .
H7 H 0.689374 0.562514 0.427768 0.026 Uiso 1 1 calc R . . . .
C9 C 0.4597(4) 0.52682(12) 0.47374(6) 0.0282(6) Uani 1 1 d . . . . .
C3 C 0.375000 0.82151(14) 0.375000 0.0282(8) Uani 1 2 d S T P . .
C4 C 0.5361(13) 0.8488(3) 0.3670(2) 0.0376(19) Uani 0.5 1 d . U . A -1
H4 H 0.648025 0.831303 0.361709 0.045 Uiso 0.5 1 calc R . . A -1
K2 K 0.625000 0.625000 0.5400(4) 0.105(8) Uani 0.140(8) 2 d S TU P B 5
C10 C 0.3307(15) 0.5256(7) 0.4967(3) 0.055(5) Uani 0.445(17) 1 d . U . C 2
H10 H 0.212537 0.542205 0.494660 0.066 Uiso 0.445(17) 1 calc R . . C 2
C12 C 0.6356(9) 0.5297(4) 0.48707(16) 0.033(2) Uani 0.555(17) 1 d . U . C 1
H12 H 0.731199 0.549825 0.478278 0.039 Uiso 0.555(17) 1 calc R . . C 1
C11 C 0.3731(14) 0.5003(7) 0.5229(2) 0.051(4) Uani 0.445(17) 1 d . U . C 2
H11 H 0.285789 0.501542 0.538760 0.062 Uiso 0.445(17) 1 calc R . . C 2
C13 C 0.6757(9) 0.5038(4) 0.51304(16) 0.0306(19) Uani 0.555(17) 1 d . U . C 1
H13 H 0.796846 0.507060 0.521824 0.037 Uiso 0.555(17) 1 calc R . . C 1
K3 K 0.212(3) 0.6346(8) 0.5047(4) 0.154(9) Uani 0.134(6) 1 d . U . D 4
K1 K 0.278(3) 0.6328(8) 0.5387(4) 0.315(10) Uani 0.306(8) 1 d . U . E 3
C5 C 0.5346(12) 0.9018(3) 0.3668(2) 0.0378(18) Uani 0.5 1 d . U . A -1
H5 H 0.644876 0.919540 0.361010 0.045 Uiso 0.5 1 calc R . . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.949(2) 14_455 ?
Fe1 N1 1.949(2) . ?
Fe1 N2 1.944(2) 14_455 ?
Fe1 N2 1.943(2) . ?
Fe1 N3 1.966(2) 3 ?
Fe1 N3 1.966(2) 16_455 ?
N1 N1 1.360(4) 3 ?
N1 C1 1.345(3) . ?
N2 N3 1.358(3) . ?
N2 C6 1.345(3) . ?
N3 C7 1.337(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.396(3) . ?
C2 C3 1.466(5) . ?
C6 H6 0.9500 . ?
C6 C8 1.398(4) . ?
C8 C7 1.385(4) . ?
C8 C9 1.473(3) . ?
C7 H7 0.9500 . ?
C9 C10 1.387(9) . ?
C9 C12 1.387(7) . ?
C9 C11 1.393(9) 17_666 ?
C9 C13 1.393(6) 17_666 ?
C3 C4 1.398(9) . ?
C3 C5 1.384(9) 2_565 ?
C4 H4 0.9500 . ?
C4 C5 1.406(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.397(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(7) . ?
C11 H11 0.9500 . ?
C13 H13 0.9500 . ?
K3 K3 1.33(4) 14_455 ?
K1 K1 4.93(5) 14 ?
C5 H5 0.9500 . ?

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
N1 Fe1 N1 179.62(12) . 14_455 ?
N1 Fe1 N3 92.89(9) . 3 ?
N1 Fe1 N3 86.84(9) 14_455 3 ?
N1 Fe1 N3 86.84(9) . 16_455 ?
N1 Fe1 N3 92.88(9) 14_455 16_455 ?
N2 Fe1 N1 90.47(9) 14_455 . ?
N2 Fe1 N1 89.79(9) . . ?
N2 Fe1 N1 89.79(9) 14_455 14_455 ?
N2 Fe1 N1 90.47(9) . 14_455 ?
N2 Fe1 N2 92.76(12) . 14_455 ?
N2 Fe1 N3 90.91(9) . 3 ?
N2 Fe1 N3 175.03(9) 14_455 3 ?
N2 Fe1 N3 175.03(9) . 16_455 ?
N2 Fe1 N3 90.92(9) 14_455 16_455 ?
N3 Fe1 N3 85.61(12) 16_455 3 ?
N1 N1 Fe1 123.67(7) 3 . ?
C1 N1 Fe1 127.64(19) . . ?
C1 N1 N1 108.02(15) . 3 ?
N3 N2 Fe1 119.67(15) . . ?
C6 N2 Fe1 132.40(18) . . ?
C6 N2 N3 107.8(2) . . ?
N2 N3 Fe1 128.47(15) . 3 ?
C7 N3 Fe1 123.29(19) . 3 ?
C7 N3 N2 108.0(2) . . ?
N1 C1 H1 124.9 . . ?
N1 C1 C2 110.3(2) . . ?
C2 C1 H1 124.9 . . ?
C1 C2 C1 103.5(3) . 3 ?
C1 C2 C3 128.27(16) . . ?
C1 C2 C3 128.27(16) 3 . ?
N2 C6 H6 125.0 . . ?
N2 C6 C8 110.0(2) . . ?
C8 C6 H6 125.0 . . ?
C6 C8 C9 131.2(3) . . ?
C7 C8 C6 103.4(2) . . ?
C7 C8 C9 125.4(3) . . ?
N3 C7 C8 110.8(2) . . ?
N3 C7 H7 124.6 . . ?
C8 C7 H7 124.6 . . ?
C10 C9 C8 122.2(4) . . ?
C12 C9 C8 120.4(3) . . ?
C12 C9 C11 38.5(6) . 17_666 ?
C12 C9 C13 117.5(4) . 17_666 ?
C11 C9 C8 120.0(4) 17_666 . ?
C13 C9 C8 122.1(3) 17_666 . ?
C13 C9 C11 103.7(6) 17_666 17_666 ?
C4 C3 C2 121.2(3) . . ?
C5 C3 C2 120.8(4) 2_565 . ?
C5 C3 C4 109.4(4) 2_565 . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.9(8) . . ?
C5 C4 H4 119.6 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(7) . . ?
C11 C10 H10 119.7 . . ?
C9 C12 H12 119.2 . . ?
C9 C12 C13 121.6(5) . . ?
C13 C12 H12 119.2 . . ?
C9 C11 C10 121.6(7) 17_666 . ?
C9 C11 H11 119.2 17_666 . ?
C10 C11 H11 119.2 . . ?
C9 C13 C12 120.8(5) 17_666 . ?
C9 C13 H13 119.6 17_666 . ?
C12 C13 H13 119.6 . . ?
H12 K3 H10 79.9 14 14_455 ?
C3 C5 C4 121.1(8) 4_565 . ?
C3 C5 H5 119.4 4_565 . ?
C4 C5 H5 119.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'







####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Na2Fe2(bdp)3
_database_code_depnum_ccdc_archive 'CCDC 2010320'
loop_
_audit_author_name
_audit_author_address
'Naomi Biggins'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-06-17 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_audit_creation_date             2019-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Na2Fe2(bdp)3
_chemical_name_systematic        Na2Fe2(bdp)3
_chemical_formula_moiety         '0.13(C288 H192 Fe16 N96), 2.06(Na)'
_chemical_formula_sum            'C36 H24 Fe2 N12 Na2.04'
_chemical_formula_weight         783.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Fe Fe 0.3511 0.8892
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
N N 0.0065 0.0035
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Na Na 0.0389 0.0265
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   7.0835(3)
_cell_length_b                   26.4668(12)
_cell_length_c                   45.398(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8511.2(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5529
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      3.35
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.947
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1569 before and 0.0879 after correction.
The Ratio of minimum to maximum transmission is 0.9092.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3187
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.021
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 100 K by an Oxford Cryosystems Cyrostream using N2 during
 the experiments. Data was collected at Beamline 12.2.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7288 angstrom) on a Bruker D8 diffractometer
equipped with a Bruker PHOTON II detector.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            25311
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.095
_diffrn_reflns_theta_min         1.840
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1767
_reflns_number_total             2180
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.692
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2180
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0568
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0914P)²+97.5342P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1747
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.

Disorder of the sodium cations required a displacement parameter restraint (SIMU) to 
prevent anisotropic refinement from resulting in elongated and enlarged thermal ellipsoids.
A linear free variable restraint (SUMP) was used on the three-component sodium cation 
disorder to restrain the sum of the occupation factors to unity. In the absence of this 
restraint, the sum of the three-component disorder was greater than one.

Additionally, disorder of the benzene rings of the ligand required displacement parameter restraints 
(SIMU).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Na3 \\sim Na1 \\sim Na2: within 2.5A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C11 \\sim C12: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C13 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C5 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 1*[Sof(Na2)]+1*[Sof(Na1)]+1*[Sof(Na3)]=1 with esd of 0.01
 Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=1-FVAR(1)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=FVAR(1)
 Fixed Sof: C5(0.5) H5(0.5) C4(0.5) H4(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C6(H6), C13(H13), C12(H12), C5(H5), C4(H4), C11(H11), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   diffmap
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 0.375000 0.375000 0.62851(2) 0.0081(2) Uani 1 2 d S T P . .
N1 N 0.2184(4) 0.43555(11) 0.62838(6) 0.0126(6) Uani 1 1 d . . . . .
N2 N 0.5394(4) 0.40522(11) 0.65804(6) 0.0123(6) Uani 1 1 d . . . . .
N3 N 0.7290(4) 0.40661(11) 0.65337(6) 0.0125(6) Uani 1 1 d . . . . .
C2 C 0.125000 0.51611(19) 0.625000 0.0169(10) Uani 1 2 d S T P . .
C1 C 0.2750(5) 0.48369(13) 0.63034(8) 0.0163(7) Uani 1 1 d . . . . .
H1 H 0.400057 0.494165 0.634769 0.020 Uiso 1 1 calc R . . . .
C3 C 0.125000 0.5716(2) 0.625000 0.0205(11) Uani 1 2 d S T P . .
C7 C 0.8073(5) 0.43084(14) 0.67598(8) 0.0165(7) Uani 1 1 d . . . . .
H7 H 0.938858 0.436918 0.678035 0.020 Uiso 1 1 calc R . . . .
C6 C 0.5042(5) 0.42844(14) 0.68355(8) 0.0181(8) Uani 1 1 d . . . . .
H6 H 0.382402 0.432452 0.691982 0.022 Uiso 1 1 calc R . . . .
C8 C 0.6719(5) 0.44599(15) 0.69608(8) 0.0187(8) Uani 1 1 d . . . . .
C9 C 0.7088(6) 0.47328(16) 0.72364(8) 0.0222(8) Uani 1 1 d . . . . .
C13 C 0.9232(12) 0.4950(4) 0.76328(19) 0.023(2) Uani 0.68(3) 1 d . U . A 2
H13 H 1.043378 0.491007 0.772280 0.027 Uiso 0.68(3) 1 calc R . . A 2
C12 C 0.8845(11) 0.4692(4) 0.73757(18) 0.023(2) Uani 0.68(3) 1 d . U . A 2
H12 H 0.978922 0.448172 0.729155 0.028 Uiso 0.68(3) 1 calc R . . A 2
C5 C 0.2824(15) 0.6513(4) 0.6175(3) 0.026(2) Uani 0.5 1 d . U . B -1
H5 H 0.393580 0.669176 0.612242 0.031 Uiso 0.5 1 calc R . . B -1
C4 C 0.2876(16) 0.5986(4) 0.6173(3) 0.027(2) Uani 0.5 1 d . U . B -1
H4 H 0.400103 0.581304 0.612034 0.032 Uiso 0.5 1 calc R . . B -1
C11 C 0.619(3) 0.5030(17) 0.7717(7) 0.056(10) Uani 0.32(3) 1 d . U . A 1
H11 H 0.525849 0.503561 0.786829 0.067 Uiso 0.32(3) 1 calc R . . A 1
C10 C 0.579(3) 0.4785(16) 0.7456(6) 0.051(9) Uani 0.32(3) 1 d . U . A 1
H10 H 0.456592 0.464794 0.742786 0.061 Uiso 0.32(3) 1 calc R . . A 1
Na3 Na 0.625000 0.625000 0.7067(3) 0.030(5) Uani 0.172(11) 2 d S TU P C 5
Na2 Na 0.215(2) 0.6123(5) 0.7443(3) 0.056(5) Uani 0.176(8) 1 d . U . D 4
Na1 Na 0.294(2) 0.6127(7) 0.7161(4) 0.115(6) Uani 0.253(9) 1 d . U . E 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.949(3) . ?
Fe1 N1 1.949(3) 2 ?
Fe1 N2 1.948(3) 2 ?
Fe1 N2 1.948(3) . ?
Fe1 N3 1.966(3) 11 ?
Fe1 N3 1.966(3) 12_455 ?
N1 N1 1.358(6) 11_455 ?
N1 C1 1.339(5) . ?
N2 N3 1.360(4) . ?
N2 C6 1.334(4) . ?
N3 C7 1.331(4) . ?
C2 C1 1.387(5) 11_455 ?
C2 C1 1.387(5) . ?
C2 C3 1.468(7) . ?
C1 H1 0.9500 . ?
C3 C4 1.400(12) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(5) . ?
C6 H6 0.9500 . ?
C6 C8 1.397(5) . ?
C8 C9 1.468(5) . ?
C9 C13 1.390(8) 25_666 ?
C9 C12 1.400(8) . ?
C9 C11 1.39(2) 25_666 ?
C9 C10 1.362(19) . ?
C13 H13 0.9500 . ?
C13 C12 1.380(10) . ?
C12 H12 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.394(10) . ?
C4 H4 0.9500 . ?
C11 H11 0.9500 . ?
C11 C10 1.38(2) . ?
C10 H10 0.9500 . ?

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
N1 Fe1 N1 179.64(16) 2 . ?
N1 Fe1 N3 92.76(12) 2 11 ?
N1 Fe1 N3 86.98(12) . 11 ?
N1 Fe1 N3 92.76(12) . 12_455 ?
N1 Fe1 N3 86.98(12) 2 12_455 ?
N2 Fe1 N1 90.28(12) . . ?
N2 Fe1 N1 90.28(12) 2 2 ?
N2 Fe1 N1 89.97(12) 2 . ?
N2 Fe1 N1 89.97(12) . 2 ?
N2 Fe1 N2 93.00(17) . 2 ?
N2 Fe1 N3 91.00(12) 2 12_455 ?
N2 Fe1 N3 174.98(12) . 12_455 ?
N2 Fe1 N3 174.98(12) 2 11 ?
N2 Fe1 N3 91.00(12) . 11 ?
N3 Fe1 N3 85.17(17) 12_455 11 ?
N1 N1 Fe1 123.72(9) 11_455 . ?
C1 N1 Fe1 127.7(3) . . ?
C1 N1 N1 107.9(2) . 11_455 ?
N3 N2 Fe1 119.6(2) . . ?
C6 N2 Fe1 132.4(3) . . ?
C6 N2 N3 107.9(3) . . ?
N2 N3 Fe1 128.5(2) . 11 ?
C7 N3 Fe1 123.6(3) . 11 ?
C7 N3 N2 107.7(3) . . ?
C1 C2 C1 103.6(5) . 11_455 ?
C1 C2 C3 128.2(2) . . ?
C1 C2 C3 128.2(2) 11_455 . ?
N1 C1 C2 110.4(3) . . ?
N1 C1 H1 124.8 . . ?
C2 C1 H1 124.8 . . ?
C4 C3 C2 120.7(5) . . ?
N3 C7 H7 124.5 . . ?
N3 C7 C8 111.0(3) . . ?
C8 C7 H7 124.5 . . ?
N2 C6 H6 124.8 . . ?
N2 C6 C8 110.3(3) . . ?
C8 C6 H6 124.8 . . ?
C7 C8 C6 103.0(3) . . ?
C7 C8 C9 125.5(4) . . ?
C6 C8 C9 131.5(4) . . ?
C13 C9 C8 122.8(4) 25_666 . ?
C13 C9 C12 116.9(5) 25_666 . ?
C13 C9 C11 104.7(11) 25_666 25_666 ?
C12 C9 C8 120.3(4) . . ?
C11 C9 C8 120.5(8) 25_666 . ?
C10 C9 C8 123.6(8) . . ?
C10 C9 C13 34.1(16) . 25_666 ?
C10 C9 C11 115.8(11) . 25_666 ?
C9 C13 H13 119.1 25_666 . ?
C12 C13 H13 119.1 . . ?
C9 C12 H12 119.3 . . ?
C13 C12 C9 121.4(6) . . ?
C13 C12 H12 119.3 . . ?
C3 C5 H5 118.4 14_455 . ?
C3 C5 C4 123.2(11) 14_455 . ?
C4 C5 H5 118.4 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(10) . . ?
C5 C4 H4 120.4 . . ?
C9 C11 H11 119.3 25_666 . ?
C10 C11 C9 121.3(17) . 25_666 ?
C10 C11 H11 119.3 . . ?
C9 C10 C11 122.7(16) . . ?
C9 C10 H10 118.6 . . ?
C11 C10 H10 118.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Li2Fe2(bdp)3
_database_code_depnum_ccdc_archive 'CCDC 2010322'
loop_
_audit_author_name
_audit_author_address
'Naomi Biggins'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_audit_creation_date             2020-07-20
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Li2Fe2(bdp)3
_chemical_name_systematic        Li2Fe2(bdp)3
_chemical_formula_moiety         '0.13(C288 H192 Fe16 N96), 2(Li)'
_chemical_formula_sum            'C36 H24 Fe2 Li2 N12'
_chemical_formula_weight         750.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
H H 0.0000 0.0000
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Fe Fe 0.3511 0.8892
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
Li Li 0.0004 0.0001
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'
N N 0.0065 0.0035
'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   7.0748(3)
_cell_length_b                   26.4454(9)
_cell_length_c                   45.3279(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8480.7(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6399
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      3.16
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1704 before and 0.0899 after correction.
The Ratio of minimum to maximum transmission is 0.8776.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tapered rod'
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.021
_exptl_special_details           
;
X-ray diffraction analyses were performed on single crystals coated with
 Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a
 temperature of 100 K by an Oxford Cryosystems Cyrostream using N2 during
 the experiments. Data was collected at Beamline 12.2.1 at the Advanced
 Light Source, Lawrence Berkeley National Laboratory using synchrotron
 radiation (lamda = 0.7288 angstrom) on a Bruker D8 diffractometer
equipped with a Bruker PHOTON II detector.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1160
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            31535
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.038
_diffrn_reflns_theta_min         3.091
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_source                   'Advanced Light Source station 12.2.1'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1597
_reflns_number_total             1957
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_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)'
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1957
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      1.156
_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)+(0.0916P)²+121.8183P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1918
_refine_special_details          
;
Thermal parameters were refined anisotropically for all non-hydrogen atoms. 
Hydrogen atoms were placed in ideal positions and refined using the riding model.

Disorder of the benzene rings of the ligand necessitated the use of displacement parameter restraints 
(SIMU and DELU).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C9, C12, C13, C10, C11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C10 \\sim C11: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C4 \\sim C5: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C9 \\sim C12 \\sim C13 \\sim C10 \\sim C11: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=1-FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=FVAR(1)
 Sof(C5)=Sof(H5)=1-FVAR(2)
 Sof(C4)=Sof(H4)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C12(H12), C13(H13), C10(H10), C11(H11), C4(H4), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.625000 0.625000 0.37142(2) 0.0071(3) Uani 1 2 d S T P . .
N1 N 0.7812(5) 0.56442(12) 0.37160(7) 0.0114(7) Uani 1 1 d . . . . .
N2 N 0.4611(5) 0.59481(12) 0.34200(7) 0.0116(7) Uani 1 1 d . . . . .
N3 N 0.2708(5) 0.59328(12) 0.34666(7) 0.0118(7) Uani 1 1 d . . . . .
C1 C 0.7244(6) 0.51659(15) 0.36967(9) 0.0151(9) Uani 1 1 d . . . . .
H1 H 0.598979 0.506236 0.365282 0.018 Uiso 1 1 calc R . . . .
C2 C 0.875000 0.4838(2) 0.375000 0.0171(13) Uani 1 2 d S T P B .
C3 C 0.875000 0.4284(2) 0.375000 0.0199(13) Uani 1 2 d S T P . .
C6 C 0.4956(6) 0.57165(16) 0.31635(9) 0.0169(9) Uani 1 1 d . . . . .
H6 H 0.617355 0.567678 0.307804 0.020 Uiso 1 1 calc R . . . .
C7 C 0.1913(6) 0.56903(16) 0.32415(9) 0.0161(9) Uani 1 1 d . . . . .
H7 H 0.059657 0.562782 0.322207 0.019 Uiso 1 1 calc R . . . .
C8 C 0.3274(6) 0.55412(18) 0.30388(9) 0.0190(10) Uani 1 1 d . . . . .
C9 C 0.2903(7) 0.52668(19) 0.27634(10) 0.0250(10) Uani 1 1 d . U . . .
C12 C 0.1139(16) 0.5298(7) 0.2628(3) 0.025(3) Uani 0.58(3) 1 d . U . A 1
H12 H 0.019166 0.550580 0.271390 0.030 Uiso 0.58(3) 1 calc R . . A 1
C13 C 0.0728(17) 0.5035(6) 0.2372(3) 0.024(3) Uani 0.58(3) 1 d . U . A 1
H13 H -0.049739 0.505946 0.228741 0.029 Uiso 0.58(3) 1 calc R . . A 1
C10 C 0.423(3) 0.5207(12) 0.2553(5) 0.037(5) Uani 0.42(3) 1 d . U . A 2
H10 H 0.546223 0.533985 0.258762 0.044 Uiso 0.42(3) 1 calc R . . A 2
C11 C 0.388(3) 0.4953(12) 0.2283(5) 0.042(6) Uani 0.42(3) 1 d . U . A 2
H11 H 0.482694 0.493201 0.213542 0.051 Uiso 0.42(3) 1 calc R . . A 2
C4 C 0.713(3) 0.4015(8) 0.3805(8) 0.034(4) Uani 0.57(6) 1 d . U . B -1
H4 H 0.597599 0.419208 0.383255 0.041 Uiso 0.57(6) 1 calc R . . B -1
C5 C 0.714(3) 0.3496(10) 0.3823(9) 0.029(5) Uani 0.43(6) 1 d . U . B -1
H5 H 0.603543 0.332399 0.388570 0.034 Uiso 0.43(6) 1 calc R . . B -1
Li1 Li 0.375000 0.375000 0.2892(7) 0.115(10) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.946(3) . ?
Fe1 N1 1.946(3) 14 ?
Fe1 N2 1.939(3) . ?
Fe1 N2 1.939(3) 14 ?
Fe1 N3 1.965(3) 3 ?
Fe1 N3 1.965(3) 16 ?
N1 N1 1.362(7) 3_655 ?
N1 C1 1.330(5) . ?
N2 N3 1.363(5) . ?
N2 C6 1.337(5) . ?
N3 C7 1.330(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.395(6) . ?
C2 C3 1.465(9) . ?
C3 C4 1.370(19) . ?
C3 C5 1.40(2) 2_655 ?
C6 H6 0.9500 . ?
C6 C8 1.397(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(6) . ?
C8 C9 1.467(6) . ?
C9 C12 1.393(11) . ?
C9 C13 1.396(11) 25_565 ?
C9 C10 1.349(17) . ?
C9 C11 1.402(17) 25_565 ?
C12 H12 0.9500 . ?
C12 C13 1.385(13) . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.42(2) . ?
C11 H11 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.377(13) . ?
C5 H5 0.9500 . ?

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
N1 Fe1 N1 179.52(19) 14 . ?
N1 Fe1 N3 92.87(14) 14 3 ?
N1 Fe1 N3 86.77(14) . 3 ?
N1 Fe1 N3 86.78(14) 14 16 ?
N1 Fe1 N3 92.87(14) . 16 ?
N2 Fe1 N1 90.12(14) . 14 ?
N2 Fe1 N1 90.20(14) 14 14 ?
N2 Fe1 N1 90.20(14) . . ?
N2 Fe1 N1 90.13(14) 14 . ?
N2 Fe1 N2 93.1(2) 14 . ?
N2 Fe1 N3 174.92(14) 14 3 ?
N2 Fe1 N3 90.95(14) . 3 ?
N2 Fe1 N3 90.95(14) 14 16 ?
N2 Fe1 N3 174.92(14) . 16 ?
N3 Fe1 N3 85.19(19) 16 3 ?
N1 N1 Fe1 123.65(11) 3_655 . ?
C1 N1 Fe1 127.7(3) . . ?
C1 N1 N1 108.0(2) . 3_655 ?
N3 N2 Fe1 119.7(2) . . ?
C6 N2 Fe1 132.7(3) . . ?
C6 N2 N3 107.6(3) . . ?
N2 N3 Fe1 128.3(2) . 3 ?
C7 N3 Fe1 123.3(3) . 3 ?
C7 N3 N2 108.2(3) . . ?
N1 C1 H1 124.8 . . ?
N1 C1 C2 110.5(4) . . ?
C2 C1 H1 124.8 . . ?
C1 C2 C1 103.0(5) 3_655 . ?
C1 C2 C3 128.5(3) 3_655 . ?
C1 C2 C3 128.5(3) . . ?
C4 C3 C2 121.2(8) . . ?
C4 C3 C5 111.3(8) . 2_655 ?
C5 C3 C2 122.0(11) 2_655 . ?
N2 C6 H6 124.8 . . ?
N2 C6 C8 110.4(4) . . ?
C8 C6 H6 124.8 . . ?
N3 C7 H7 124.7 . . ?
N3 C7 C8 110.6(4) . . ?
C8 C7 H7 124.7 . . ?
C6 C8 C9 131.3(4) . . ?
C7 C8 C6 103.2(4) . . ?
C7 C8 C9 125.4(4) . . ?
C12 C9 C8 120.3(6) . . ?
C12 C9 C13 117.5(7) . 25_565 ?
C12 C9 C11 32.3(10) . 25_565 ?
C13 C9 C8 122.2(6) 25_565 . ?
C13 C9 C11 108.7(9) 25_565 25_565 ?
C10 C9 C8 122.3(8) . . ?
C10 C9 C11 118.2(10) . 25_565 ?
C11 C9 C8 119.5(7) 25_565 . ?
C9 C12 H12 119.1 . . ?
C13 C12 C9 121.8(8) . . ?
C13 C12 H12 119.1 . . ?
C9 C13 H13 119.7 25_565 . ?
C12 C13 C9 120.7(9) . 25_565 ?
C12 C13 H13 119.7 . . ?
C9 C10 H10 118.7 . . ?
C9 C10 C11 122.7(13) . . ?
C11 C10 H10 118.7 . . ?
C9 C11 C10 119.0(13) 25_565 . ?
C9 C11 H11 120.5 25_565 . ?
C10 C11 H11 120.5 . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 122(2) . . ?
C5 C4 H4 119.2 . . ?
C3 C5 H5 119.3 4 . ?
C4 C5 C3 121(2) . 4 ?
C4 C5 H5 119.3 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

