# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_pr210_120k
_database_code_depnum_ccdc_archive 'CCDC 2261109'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_systematic        
bis(bis(1H-pyrazol-1-yl)(1H-3,5-dimethylpyrazol-1-yl)borohydride)iron(ii)
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7267(6)
_cell_length_b                   10.5289(7)
_cell_length_c                   12.1811(8)
_cell_angle_alpha                93.485(4)
_cell_angle_beta                 95.007(4)
_cell_angle_gamma                95.425(4)
_cell_volume                     1234.16(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4742
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.407
_shelx_estimated_absorpt_T_max   0.938
_shelx_estimated_absorpt_T_min   0.781
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂,.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9014
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         3.237
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.077629
_diffrn_orient_matrix_UB_12      -0.044408
_diffrn_orient_matrix_UB_13      0.034434
_diffrn_orient_matrix_UB_21      -0.039352
_diffrn_orient_matrix_UB_22      -0.081891
_diffrn_orient_matrix_UB_23      -0.041858
_diffrn_orient_matrix_UB_31      0.056433
_diffrn_orient_matrix_UB_32      0.021633
_diffrn_orient_matrix_UB_33      -0.062341
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by
 a combination of 3 sets of ω scans each set at different φ and/or
 2θ angles and each scan (38.00 s exposure) covering 1.900\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4525
_reflns_number_total             5621
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.038
_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)+(0.0471P)²+0.5018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0999
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.02144(10) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.02127(10) Uani 1 2 d S . P . .
N7 N 0.80991(16) 1.01349(15) 0.92858(13) 0.0249(3) Uani 1 1 d . . . . .
N2 N 0.78282(16) 0.55204(15) 0.44044(13) 0.0237(3) Uani 1 1 d . . . . .
N10 N 0.86033(16) 0.74385(15) 0.96322(13) 0.0245(3) Uani 1 1 d . . . . .
N8 N 0.70653(16) 0.91806(15) 0.94210(13) 0.0241(3) Uani 1 1 d . . . . .
N1 N 0.69401(16) 0.58739(15) 0.51651(13) 0.0231(3) Uani 1 1 d . . . . .
N11 N 0.91395(16) 0.95694(15) 1.13549(13) 0.0239(3) Uani 1 1 d . . . . .
N6 N 0.60540(16) 0.48918(15) 0.28419(13) 0.0243(3) Uani 1 1 d . . . . .
N5 N 0.49610(16) 0.51986(15) 0.33946(13) 0.0241(3) Uani 1 1 d . . . . .
N4 N 0.67863(16) 0.32503(15) 0.40930(13) 0.0246(3) Uani 1 1 d . . . . .
N12 N 0.80144(16) 0.86769(15) 1.12920(13) 0.0243(3) Uani 1 1 d . . . . .
N9 N 0.97892(16) 0.81801(15) 0.94689(13) 0.0242(3) Uani 1 1 d . . . . .
N3 N 0.57970(16) 0.33616(15) 0.48115(13) 0.0246(3) Uani 1 1 d . . . . .
C14 C 0.5863(2) 0.9410(2) 0.88457(16) 0.0272(4) Uani 1 1 d . . . . .
C13 C 0.6120(2) 1.0519(2) 0.83366(17) 0.0305(4) Uani 1 1 d . . . . .
H13 H 0.547577 1.091689 0.787448 0.037 Uiso 1 1 calc R U . . .
C12 C 0.7520(2) 1.09546(19) 0.86290(16) 0.0274(4) Uani 1 1 d . . . . .
C4 C 0.5563(2) 0.22140(19) 0.52102(17) 0.0289(4) Uani 1 1 d . . . . .
H4 H 0.492207 0.201492 0.573516 0.035 Uiso 1 1 calc R U . . .
C6 C 0.7144(2) 0.20465(19) 0.40404(18) 0.0295(4) Uani 1 1 d . . . . .
H6 H 0.780452 0.172854 0.359192 0.035 Uiso 1 1 calc R U . . .
C17 C 0.8708(2) 0.62212(19) 0.92727(17) 0.0287(4) Uani 1 1 d . . . . .
H17 H 0.802055 0.552223 0.929839 0.034 Uiso 1 1 calc R U . . .
C5 C 0.6388(2) 0.1350(2) 0.47503(19) 0.0332(5) Uani 1 1 d . . . . .
H5 H 0.642270 0.047630 0.489263 0.040 Uiso 1 1 calc R U . . .
C3 C 0.90318(19) 0.62883(19) 0.45595(16) 0.0255(4) Uani 1 1 d . . . . .
C15 C 1.0610(2) 0.74097(19) 0.90006(17) 0.0287(4) Uani 1 1 d . . . . .
H15 H 1.150491 0.767402 0.878967 0.034 Uiso 1 1 calc R U . . .
C1 C 0.7622(2) 0.68466(19) 0.58082(16) 0.0257(4) Uani 1 1 d . . . . .
C2 C 0.8943(2) 0.71341(19) 0.54459(17) 0.0282(4) Uani 1 1 d . . . . .
H2 H 0.963632 0.778506 0.575428 0.034 Uiso 1 1 calc R U . . .
C16 C 0.9973(2) 0.6156(2) 0.88619(18) 0.0316(4) Uani 1 1 d . . . . .
H16 H 1.033485 0.542197 0.855237 0.038 Uiso 1 1 calc R U . . .
C18 C 0.9475(2) 0.98991(19) 1.24259(16) 0.0271(4) Uani 1 1 d . . . . .
H18 H 1.021919 1.051211 1.271231 0.032 Uiso 1 1 calc R U . . .
C7 C 0.4073(2) 0.5663(2) 0.26613(17) 0.0289(4) Uani 1 1 d . . . . .
H7 H 0.320742 0.594501 0.281855 0.035 Uiso 1 1 calc R U . . .
C20 C 0.7672(2) 0.84514(19) 1.23133(16) 0.0274(4) Uani 1 1 d . . . . .
H20 H 0.693173 0.786464 1.248589 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5853(2) 0.5182(2) 0.17804(16) 0.0294(4) Uani 1 1 d . . . . .
H9 H 0.647379 0.506306 0.123111 0.035 Uiso 1 1 calc R U . . .
C19 C 0.8579(2) 0.9217(2) 1.30696(17) 0.0299(4) Uani 1 1 d . . . . .
H19 H 0.859178 0.926952 1.385179 0.036 Uiso 1 1 calc R U . . .
C21 C 0.8290(2) 1.2140(2) 0.8301(2) 0.0380(5) Uani 1 1 d . . . . .
H21A H 0.799096 1.288621 0.870111 0.057 Uiso 1 1 calc R U . . .
H21B H 0.809954 1.220767 0.750439 0.057 Uiso 1 1 calc R U . . .
H21C H 0.928769 1.210820 0.848147 0.057 Uiso 1 1 calc R U . . .
C8 C 0.4599(2) 0.5677(2) 0.16273(17) 0.0314(4) Uani 1 1 d . . . . .
H8 H 0.418021 0.596539 0.096601 0.038 Uiso 1 1 calc R U . . .
C22 C 0.4550(2) 0.8543(2) 0.88208(19) 0.0377(5) Uani 1 1 d . . . . .
H22A H 0.467241 0.771206 0.845534 0.057 Uiso 1 1 calc R U . . .
H22B H 0.379582 0.892297 0.841260 0.057 Uiso 1 1 calc R U . . .
H22C H 0.431961 0.842754 0.957805 0.057 Uiso 1 1 calc R U . . .
C10 C 0.7041(2) 0.7505(2) 0.67536(18) 0.0335(5) Uani 1 1 d . . . . .
H10A H 0.688817 0.838026 0.657941 0.050 Uiso 1 1 calc R U . . .
H10B H 0.769494 0.752892 0.741553 0.050 Uiso 1 1 calc R U . . .
H10C H 0.615745 0.703944 0.688814 0.050 Uiso 1 1 calc R U . . .
C11 C 1.0177(2) 0.6176(2) 0.38180(18) 0.0323(4) Uani 1 1 d . . . . .
H11A H 1.041821 0.529283 0.377566 0.048 Uiso 1 1 calc R U . . .
H11B H 1.099235 0.675074 0.411740 0.048 Uiso 1 1 calc R U . . .
H11C H 0.986619 0.641163 0.307739 0.048 Uiso 1 1 calc R U . . .
B1 B 0.7317(2) 0.4439(2) 0.35163(18) 0.0259(4) Uani 1 1 d . . . . .
B2 B 0.7423(2) 0.8088(2) 1.01363(18) 0.0246(4) Uani 1 1 d . . . . .
H1 H 0.811(2) 0.423(2) 0.2957(18) 0.029(6) Uiso 1 1 d . . . . .
H2A H 0.653(2) 0.738(2) 1.019(2) 0.036(6) Uiso 1 1 d . . . . .


_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 2.0077(15) . ?
Fe01 N1 2.0077(15) 2_666 ?
Fe01 N5 1.9768(16) . ?
Fe01 N5 1.9768(16) 2_666 ?
Fe01 N3 1.9660(16) . ?
Fe01 N3 1.9660(16) 2_666 ?
Fe02 N7 1.9949(16) 2_777 ?
Fe02 N7 1.9948(16) . ?
Fe02 N11 1.9724(16) 2_777 ?
Fe02 N11 1.9724(16) . ?
Fe02 N9 1.9708(16) 2_777 ?
Fe02 N9 1.9708(16) . ?
N7 N8 1.380(2) . ?
N7 C12 1.341(2) . ?
N2 N1 1.379(2) . ?
N2 C3 1.350(2) . ?
N2 B1 1.537(3) . ?
N10 N9 1.367(2) . ?
N10 C17 1.345(3) . ?
N10 B2 1.544(3) . ?
N8 C14 1.359(2) . ?
N8 B2 1.532(3) . ?
N1 C1 1.336(2) . ?
N11 N12 1.367(2) . ?
N11 C18 1.333(3) . ?
N6 N5 1.361(2) . ?
N6 C9 1.348(3) . ?
N6 B1 1.547(3) . ?
N5 C7 1.335(3) . ?
N4 N3 1.364(2) . ?
N4 C6 1.345(3) . ?
N4 B1 1.541(3) . ?
N12 C20 1.345(2) . ?
N12 B2 1.543(3) . ?
N9 C15 1.329(3) . ?
N3 C4 1.337(2) . ?
C14 C13 1.367(3) . ?
C14 C22 1.495(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.403(3) . ?
C12 C21 1.489(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.383(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.375(3) . ?
C5 H5 0.9500 . ?
C3 C2 1.371(3) . ?
C3 C11 1.502(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.398(3) . ?
C1 C2 1.407(3) . ?
C1 C10 1.489(3) . ?
C2 H2 0.9500 . ?
C16 H16 0.9500 . ?
C18 H18 0.9500 . ?
C18 C19 1.399(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.400(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.382(3) . ?
C9 H9 0.9500 . ?
C9 C8 1.374(3) . ?
C19 H19 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C8 H8 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
B1 H1 1.10(2) . ?
B2 H2A 1.10(2) . ?

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 180.0 2_666 . ?
N5 Fe01 N1 91.78(6) . 2_666 ?
N5 Fe01 N1 91.78(6) 2_666 . ?
N5 Fe01 N1 88.22(6) 2_666 2_666 ?
N5 Fe01 N1 88.22(6) . . ?
N5 Fe01 N5 180.00(9) 2_666 . ?
N3 Fe01 N1 91.86(6) . 2_666 ?
N3 Fe01 N1 88.14(6) 2_666 2_666 ?
N3 Fe01 N1 91.86(6) 2_666 . ?
N3 Fe01 N1 88.14(6) . . ?
N3 Fe01 N5 90.49(7) 2_666 2_666 ?
N3 Fe01 N5 90.49(7) . . ?
N3 Fe01 N5 89.51(7) . 2_666 ?
N3 Fe01 N5 89.51(7) 2_666 . ?
N3 Fe01 N3 180.0 . 2_666 ?
N7 Fe02 N7 180.0 . 2_777 ?
N11 Fe02 N7 92.10(6) . 2_777 ?
N11 Fe02 N7 87.90(6) 2_777 2_777 ?
N11 Fe02 N7 92.10(6) 2_777 . ?
N11 Fe02 N7 87.90(6) . . ?
N11 Fe02 N11 180.0 . 2_777 ?
N9 Fe02 N7 88.22(7) . . ?
N9 Fe02 N7 91.78(7) . 2_777 ?
N9 Fe02 N7 91.78(7) 2_777 . ?
N9 Fe02 N7 88.22(7) 2_777 2_777 ?
N9 Fe02 N11 90.46(7) 2_777 2_777 ?
N9 Fe02 N11 89.54(7) . 2_777 ?
N9 Fe02 N11 90.46(7) . . ?
N9 Fe02 N11 89.54(7) 2_777 . ?
N9 Fe02 N9 180.0 . 2_777 ?
N8 N7 Fe02 118.33(12) . . ?
C12 N7 Fe02 135.20(13) . . ?
C12 N7 N8 106.43(15) . . ?
N1 N2 B1 118.90(15) . . ?
C3 N2 N1 110.12(15) . . ?
C3 N2 B1 130.86(16) . . ?
N9 N10 B2 118.42(15) . . ?
C17 N10 N9 109.49(16) . . ?
C17 N10 B2 132.07(16) . . ?
N7 N8 B2 118.48(15) . . ?
C14 N8 N7 109.93(16) . . ?
C14 N8 B2 131.58(16) . . ?
N2 N1 Fe01 117.68(11) . . ?
C1 N1 Fe01 135.51(14) . . ?
C1 N1 N2 106.54(15) . . ?
N12 N11 Fe02 119.77(12) . . ?
C18 N11 Fe02 133.59(13) . . ?
C18 N11 N12 106.42(15) . . ?
N5 N6 B1 117.89(15) . . ?
C9 N6 N5 109.85(16) . . ?
C9 N6 B1 131.87(17) . . ?
N6 N5 Fe01 119.78(12) . . ?
C7 N5 Fe01 133.61(14) . . ?
C7 N5 N6 106.49(16) . . ?
N3 N4 B1 118.90(16) . . ?
C6 N4 N3 109.85(16) . . ?
C6 N4 B1 131.24(17) . . ?
N11 N12 B2 117.76(15) . . ?
C20 N12 N11 109.87(16) . . ?
C20 N12 B2 132.31(16) . . ?
N10 N9 Fe02 119.12(12) . . ?
C15 N9 Fe02 134.16(13) . . ?
C15 N9 N10 106.61(16) . . ?
N4 N3 Fe01 118.99(12) . . ?
C4 N3 Fe01 134.58(14) . . ?
C4 N3 N4 106.37(16) . . ?
N8 C14 C13 107.49(17) . . ?
N8 C14 C22 122.90(18) . . ?
C13 C14 C22 129.61(19) . . ?
C14 C13 H13 126.6 . . ?
C14 C13 C12 106.72(17) . . ?
C12 C13 H13 126.6 . . ?
N7 C12 C13 109.43(17) . . ?
N7 C12 C21 123.26(18) . . ?
C13 C12 C21 127.30(18) . . ?
N3 C4 H4 124.7 . . ?
N3 C4 C5 110.66(18) . . ?
C5 C4 H4 124.7 . . ?
N4 C6 H6 125.8 . . ?
N4 C6 C5 108.37(18) . . ?
C5 C6 H6 125.8 . . ?
N10 C17 H17 125.7 . . ?
N10 C17 C16 108.68(17) . . ?
C16 C17 H17 125.7 . . ?
C4 C5 H5 127.6 . . ?
C6 C5 C4 104.74(18) . . ?
C6 C5 H5 127.6 . . ?
N2 C3 C2 107.57(17) . . ?
N2 C3 C11 122.33(18) . . ?
C2 C3 C11 130.07(18) . . ?
N9 C15 H15 124.7 . . ?
N9 C15 C16 110.51(18) . . ?
C16 C15 H15 124.7 . . ?
N1 C1 C2 109.38(18) . . ?
N1 C1 C10 124.13(17) . . ?
C2 C1 C10 126.50(18) . . ?
C3 C2 C1 106.37(17) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C17 C16 C15 104.71(18) . . ?
C17 C16 H16 127.6 . . ?
C15 C16 H16 127.6 . . ?
N11 C18 H18 124.7 . . ?
N11 C18 C19 110.63(18) . . ?
C19 C18 H18 124.7 . . ?
N5 C7 H7 124.8 . . ?
N5 C7 C8 110.41(18) . . ?
C8 C7 H7 124.8 . . ?
N12 C20 H20 125.8 . . ?
N12 C20 C19 108.48(17) . . ?
C19 C20 H20 125.8 . . ?
N6 C9 H9 125.8 . . ?
N6 C9 C8 108.48(18) . . ?
C8 C9 H9 125.8 . . ?
C18 C19 H19 127.7 . . ?
C20 C19 C18 104.60(18) . . ?
C20 C19 H19 127.7 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.6 . . ?
C9 C8 C7 104.76(18) . . ?
C9 C8 H8 127.6 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 106.39(16) . . ?
N2 B1 N4 108.60(16) . . ?
N2 B1 H1 113.0(11) . . ?
N6 B1 H1 109.2(11) . . ?
N4 B1 N6 107.24(15) . . ?
N4 B1 H1 112.2(11) . . ?
N10 B2 H2A 110.1(13) . . ?
N8 B2 N10 107.81(15) . . ?
N8 B2 N12 108.11(16) . . ?
N8 B2 H2A 112.5(13) . . ?
N12 B2 N10 106.77(15) . . ?
N12 B2 H2A 111.4(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -172.50(14) . . . . ?
Fe01 N1 C1 C10 7.4(3) . . . . ?
Fe01 N5 C7 C8 175.17(14) . . . . ?
Fe01 N3 C4 C5 176.63(15) . . . . ?
Fe02 N7 N8 C14 -177.75(13) . . . . ?
Fe02 N7 N8 B2 1.6(2) . . . . ?
Fe02 N7 C12 C13 177.13(15) . . . . ?
Fe02 N7 C12 C21 -3.7(3) . . . . ?
Fe02 N11 N12 C20 174.68(13) . . . . ?
Fe02 N11 N12 B2 -2.9(2) . . . . ?
Fe02 N11 C18 C19 -173.91(14) . . . . ?
Fe02 N9 C15 C16 175.44(15) . . . . ?
N7 N8 C14 C13 -0.1(2) . . . . ?
N7 N8 C14 C22 179.68(18) . . . . ?
N7 N8 B2 N10 -58.3(2) . . . . ?
N7 N8 B2 N12 56.7(2) . . . . ?
N2 N1 C1 C2 1.1(2) . . . . ?
N2 N1 C1 C10 -179.05(18) . . . . ?
N2 C3 C2 C1 -0.7(2) . . . . ?
N10 N9 C15 C16 -0.5(2) . . . . ?
N10 C17 C16 C15 0.0(2) . . . . ?
N8 N7 C12 C13 -0.5(2) . . . . ?
N8 N7 C12 C21 178.67(19) . . . . ?
N8 C14 C13 C12 -0.2(2) . . . . ?
N1 N2 C3 C2 1.4(2) . . . . ?
N1 N2 C3 C11 -176.91(17) . . . . ?
N1 N2 B1 N6 60.6(2) . . . . ?
N1 N2 B1 N4 -54.5(2) . . . . ?
N1 C1 C2 C3 -0.3(2) . . . . ?
N11 N12 C20 C19 0.6(2) . . . . ?
N11 N12 B2 N10 59.5(2) . . . . ?
N11 N12 B2 N8 -56.3(2) . . . . ?
N11 C18 C19 C20 -0.1(2) . . . . ?
N6 N5 C7 C8 -0.8(2) . . . . ?
N6 C9 C8 C7 0.1(2) . . . . ?
N5 N6 C9 C8 -0.6(2) . . . . ?
N5 N6 B1 N2 -57.8(2) . . . . ?
N5 N6 B1 N4 58.3(2) . . . . ?
N5 C7 C8 C9 0.5(2) . . . . ?
N4 N3 C4 C5 -0.4(2) . . . . ?
N4 C6 C5 C4 0.5(2) . . . . ?
N12 N11 C18 C19 0.5(2) . . . . ?
N12 C20 C19 C18 -0.2(2) . . . . ?
N9 N10 C17 C16 -0.3(2) . . . . ?
N9 N10 B2 N8 54.8(2) . . . . ?
N9 N10 B2 N12 -61.2(2) . . . . ?
N9 C15 C16 C17 0.3(2) . . . . ?
N3 N4 C6 C5 -0.8(2) . . . . ?
N3 N4 B1 N2 54.6(2) . . . . ?
N3 N4 B1 N6 -60.0(2) . . . . ?
N3 C4 C5 C6 0.0(2) . . . . ?
C14 N8 B2 N10 120.8(2) . . . . ?
C14 N8 B2 N12 -124.1(2) . . . . ?
C14 C13 C12 N7 0.5(2) . . . . ?
C14 C13 C12 C21 -178.7(2) . . . . ?
C12 N7 N8 C14 0.4(2) . . . . ?
C12 N7 N8 B2 179.68(17) . . . . ?
C6 N4 N3 Fe01 -176.86(13) . . . . ?
C6 N4 N3 C4 0.7(2) . . . . ?
C6 N4 B1 N2 -124.0(2) . . . . ?
C6 N4 B1 N6 121.4(2) . . . . ?
C17 N10 N9 Fe02 -176.18(13) . . . . ?
C17 N10 N9 C15 0.5(2) . . . . ?
C17 N10 B2 N8 -123.4(2) . . . . ?
C17 N10 B2 N12 120.6(2) . . . . ?
C3 N2 N1 Fe01 173.40(12) . . . . ?
C3 N2 N1 C1 -1.5(2) . . . . ?
C3 N2 B1 N6 -115.1(2) . . . . ?
C3 N2 B1 N4 129.8(2) . . . . ?
C18 N11 N12 C20 -0.6(2) . . . . ?
C18 N11 N12 B2 -178.18(17) . . . . ?
C20 N12 B2 N10 -117.4(2) . . . . ?
C20 N12 B2 N8 126.9(2) . . . . ?
C9 N6 N5 Fe01 -175.80(12) . . . . ?
C9 N6 N5 C7 0.9(2) . . . . ?
C9 N6 B1 N2 114.2(2) . . . . ?
C9 N6 B1 N4 -129.7(2) . . . . ?
C22 C14 C13 C12 -180.0(2) . . . . ?
C10 C1 C2 C3 179.9(2) . . . . ?
C11 C3 C2 C1 177.4(2) . . . . ?
B1 N2 N1 Fe01 -3.1(2) . . . . ?
B1 N2 N1 C1 -178.05(17) . . . . ?
B1 N2 C3 C2 177.33(19) . . . . ?
B1 N2 C3 C11 -0.9(3) . . . . ?
B1 N6 N5 Fe01 -2.1(2) . . . . ?
B1 N6 N5 C7 174.56(17) . . . . ?
B1 N6 C9 C8 -173.08(19) . . . . ?
B1 N4 N3 Fe01 4.2(2) . . . . ?
B1 N4 N3 C4 -178.20(17) . . . . ?
B1 N4 C6 C5 177.98(19) . . . . ?
B2 N10 N9 Fe02 5.3(2) . . . . ?
B2 N10 N9 C15 -178.07(17) . . . . ?
B2 N10 C17 C16 177.99(19) . . . . ?
B2 N8 C14 C13 -179.26(19) . . . . ?
B2 N8 C14 C22 0.5(3) . . . . ?
B2 N12 C20 C19 177.61(19) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_120K
_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_pr210_250k
_database_code_depnum_ccdc_archive 'CCDC 2261110'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
bis(bis(1H-pyrazol-1-yl)(1H-3,5-dimethylpyrazol-1-yl)borohydride)iron(ii)
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8079(3)
_cell_length_b                   10.6387(3)
_cell_length_c                   12.2147(3)
_cell_angle_alpha                93.176(2)
_cell_angle_beta                 94.880(2)
_cell_angle_gamma                95.584(2)
_cell_volume                     1261.27(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5760
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_cell_measurement_wavelength     0.71073
_shelx_estimated_absorpt_T_max   0.939
_shelx_estimated_absorpt_T_min   0.785
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂,.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0127
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10381
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         3.212
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.07767
_diffrn_orient_matrix_UB_12      -0.017384
_diffrn_orient_matrix_UB_13      0.053658
_diffrn_orient_matrix_UB_21      -0.01103
_diffrn_orient_matrix_UB_22      -0.0908
_diffrn_orient_matrix_UB_23      -0.028206
_diffrn_orient_matrix_UB_31      0.066545
_diffrn_orient_matrix_UB_32      0.020244
_diffrn_orient_matrix_UB_33      -0.055718
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 10 sets of ω scans each set at different φ and/or  2θ angles and each scan (114.00 s exposure) covering 1.900\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4897
_reflns_number_total             5761
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5761
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0380
_refine_ls_restrained_S_all      1.057
_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)+(0.0631P)²+0.2910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1072
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.03455(10) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.03463(10) Uani 1 2 d S . P . .
N7 N 0.81072(14) 1.01100(14) 0.92764(12) 0.0407(3) Uani 1 1 d . . . . .
N2 N 0.78050(14) 0.55309(14) 0.43909(12) 0.0390(3) Uani 1 1 d . . . . .
N10 N 0.86354(15) 0.74541(14) 0.96447(12) 0.0418(3) Uani 1 1 d . . . . .
N8 N 0.70912(14) 0.91587(14) 0.94252(12) 0.0414(3) Uani 1 1 d . . . . .
N1 N 0.69258(14) 0.58775(14) 0.51524(11) 0.0386(3) Uani 1 1 d . . . . .
N11 N 0.91368(15) 0.95704(13) 1.13552(12) 0.0397(3) Uani 1 1 d . . . . .
N6 N 0.60391(15) 0.48997(14) 0.28429(12) 0.0418(3) Uani 1 1 d . . . . .
N5 N 0.49532(15) 0.51917(14) 0.33919(12) 0.0403(3) Uani 1 1 d . . . . .
N4 N 0.67834(15) 0.32829(14) 0.40969(12) 0.0421(3) Uani 1 1 d . . . . .
N12 N 0.80306(15) 0.86764(14) 1.12910(12) 0.0407(3) Uani 1 1 d . . . . .
N9 N 0.98054(15) 0.81950(13) 0.94848(12) 0.0405(3) Uani 1 1 d . . . . .
N3 N 0.58047(15) 0.33805(14) 0.48147(12) 0.0412(3) Uani 1 1 d . . . . .
C14 C 0.58972(18) 0.93711(19) 0.88521(15) 0.0469(4) Uani 1 1 d . . . . .
C13 C 0.6141(2) 1.0467(2) 0.83337(17) 0.0538(5) Uani 1 1 d . . . . .
H13 H 0.550471 1.084884 0.787516 0.065 Uiso 1 1 calc R U . . .
C12 C 0.75273(19) 1.09108(19) 0.86196(16) 0.0472(4) Uani 1 1 d . . . . .
C4 C 0.5587(2) 0.22454(18) 0.52183(17) 0.0500(4) Uani 1 1 d . . . . .
H4 H 0.496369 0.204362 0.574125 0.060 Uiso 1 1 calc R U . . .
C6 C 0.7150(2) 0.20938(18) 0.40499(18) 0.0514(4) Uani 1 1 d . . . . .
H6 H 0.780140 0.178868 0.360861 0.062 Uiso 1 1 calc R U . . .
C17 C 0.8747(2) 0.62558(18) 0.92910(17) 0.0508(4) Uani 1 1 d . . . . .
H17 H 0.807553 0.556776 0.931893 0.061 Uiso 1 1 calc R U . . .
C5 C 0.6408(2) 0.14037(19) 0.4758(2) 0.0591(5) Uani 1 1 d . . . . .
H5 H 0.644780 0.054799 0.490017 0.071 Uiso 1 1 calc R U . . .
C3 C 0.90031(18) 0.62870(17) 0.45431(15) 0.0423(4) Uani 1 1 d . . . . .
C15 C 1.0628(2) 0.74377(18) 0.90196(17) 0.0502(4) Uani 1 1 d . . . . .
H15 H 1.150687 0.770255 0.881336 0.060 Uiso 1 1 calc R U . . .
C1 C 0.76090(19) 0.68368(17) 0.57888(15) 0.0428(4) Uani 1 1 d . . . . .
C2 C 0.89133(19) 0.71174(18) 0.54277(16) 0.0476(4) Uani 1 1 d . . . . .
H2 H 0.959574 0.775175 0.573207 0.057 Uiso 1 1 calc R U . . .
C16 C 1.0003(2) 0.61969(19) 0.88812(18) 0.0559(5) Uani 1 1 d . . . . .
H16 H 1.036005 0.548165 0.857612 0.067 Uiso 1 1 calc R U . . .
C18 C 0.9441(2) 0.99153(18) 1.24178(15) 0.0472(4) Uani 1 1 d . . . . .
H18 H 1.015726 1.052895 1.270089 0.057 Uiso 1 1 calc R U . . .
C7 C 0.4066(2) 0.56340(19) 0.26614(16) 0.0484(4) Uani 1 1 d . . . . .
H7 H 0.321206 0.589945 0.281625 0.058 Uiso 1 1 calc R U . . .
C20 C 0.7675(2) 0.84651(18) 1.23108(16) 0.0478(4) Uani 1 1 d . . . . .
H20 H 0.695106 0.788608 1.248481 0.057 Uiso 1 1 calc R U . . .
C9 C 0.5830(2) 0.51780(19) 0.17837(15) 0.0501(4) Uani 1 1 d . . . . .
H9 H 0.643777 0.506817 0.123956 0.060 Uiso 1 1 calc R U . . .
C19 C 0.8548(2) 0.9239(2) 1.30515(16) 0.0534(5) Uani 1 1 d . . . . .
H19 H 0.854537 0.929927 1.382200 0.064 Uiso 1 1 calc R U . . .
C21 C 0.8278(2) 1.2082(2) 0.8273(2) 0.0658(6) Uani 1 1 d . . . . .
H21A H 0.797944 1.281372 0.865877 0.099 Uiso 1 1 calc R U . . .
H21B H 0.808674 1.213619 0.748589 0.099 Uiso 1 1 calc R U . . .
H21C H 0.925865 1.206083 0.844872 0.099 Uiso 1 1 calc R U . . .
C8 C 0.4583(2) 0.5648(2) 0.16333(17) 0.0560(5) Uani 1 1 d . . . . .
H8 H 0.416503 0.592011 0.097905 0.067 Uiso 1 1 calc R U . . .
C22 C 0.4598(2) 0.8508(3) 0.8842(2) 0.0644(6) Uani 1 1 d . . . . .
H22A H 0.470712 0.770406 0.846133 0.097 Uiso 1 1 calc R U . . .
H22B H 0.384603 0.888879 0.846553 0.097 Uiso 1 1 calc R U . . .
H22C H 0.439771 0.837004 0.959287 0.097 Uiso 1 1 calc R U . . .
C10 C 0.7037(2) 0.7483(2) 0.67315(17) 0.0559(5) Uani 1 1 d . . . . .
H10A H 0.688374 0.833999 0.655770 0.084 Uiso 1 1 calc R U . . .
H10B H 0.768144 0.750783 0.738195 0.084 Uiso 1 1 calc R U . . .
H10C H 0.617112 0.702364 0.686982 0.084 Uiso 1 1 calc R U . . .
C11 C 1.0145(2) 0.6170(2) 0.38118(18) 0.0538(5) Uani 1 1 d . . . . .
H11A H 1.039156 0.530796 0.379178 0.081 Uiso 1 1 calc R U . . .
H11B H 1.093907 0.674535 0.409753 0.081 Uiso 1 1 calc R U . . .
H11C H 0.984221 0.637932 0.307350 0.081 Uiso 1 1 calc R U . . .
B1 B 0.7293(2) 0.4458(2) 0.35130(16) 0.0421(4) Uani 1 1 d . . . . .
B2 B 0.7460(2) 0.80865(19) 1.01437(17) 0.0416(4) Uani 1 1 d . . . . .
H1 H 0.807(2) 0.4290(19) 0.2953(16) 0.045(5) Uiso 1 1 d . . . . .
H2A H 0.659(2) 0.738(2) 1.0201(17) 0.047(5) Uiso 1 1 d . . . . .


_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 2.0128(14) 2_666 ?
Fe01 N1 2.0128(14) . ?
Fe01 N5 1.9831(14) 2_666 ?
Fe01 N5 1.9831(14) . ?
Fe01 N3 1.9734(15) 2_666 ?
Fe01 N3 1.9735(15) . ?
Fe02 N7 2.0039(14) . ?
Fe02 N7 2.0039(14) 2_777 ?
Fe02 N11 1.9780(14) 2_777 ?
Fe02 N11 1.9780(14) . ?
Fe02 N9 1.9734(15) . ?
Fe02 N9 1.9733(15) 2_777 ?
N7 N8 1.380(2) . ?
N7 C12 1.336(2) . ?
N2 N1 1.3802(19) . ?
N2 C3 1.351(2) . ?
N2 B1 1.538(2) . ?
N10 N9 1.3622(19) . ?
N10 C17 1.341(2) . ?
N10 B2 1.542(2) . ?
N8 C14 1.357(2) . ?
N8 B2 1.530(3) . ?
N1 C1 1.336(2) . ?
N11 N12 1.365(2) . ?
N11 C18 1.330(2) . ?
N6 N5 1.358(2) . ?
N6 C9 1.346(2) . ?
N6 B1 1.545(3) . ?
N5 C7 1.330(2) . ?
N4 N3 1.361(2) . ?
N4 C6 1.348(2) . ?
N4 B1 1.536(3) . ?
N12 C20 1.347(2) . ?
N12 B2 1.540(3) . ?
N9 C15 1.333(2) . ?
N3 C4 1.334(2) . ?
C14 C13 1.368(3) . ?
C14 C22 1.495(3) . ?
C13 H13 0.9400 . ?
C13 C12 1.403(3) . ?
C12 C21 1.486(3) . ?
C4 H4 0.9400 . ?
C4 C5 1.388(3) . ?
C6 H6 0.9400 . ?
C6 C5 1.375(3) . ?
C17 H17 0.9400 . ?
C17 C16 1.374(3) . ?
C5 H5 0.9400 . ?
C3 C2 1.372(3) . ?
C3 C11 1.501(3) . ?
C15 H15 0.9400 . ?
C15 C16 1.395(3) . ?
C1 C2 1.399(3) . ?
C1 C10 1.487(3) . ?
C2 H2 0.9400 . ?
C16 H16 0.9400 . ?
C18 H18 0.9400 . ?
C18 C19 1.392(3) . ?
C7 H7 0.9400 . ?
C7 C8 1.394(3) . ?
C20 H20 0.9400 . ?
C20 C19 1.370(3) . ?
C9 H9 0.9400 . ?
C9 C8 1.367(3) . ?
C19 H19 0.9400 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C8 H8 0.9400 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
B1 H1 1.09(2) . ?
B2 H2A 1.09(2) . ?

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 180.0 . 2_666 ?
N5 Fe01 N1 91.73(6) 2_666 . ?
N5 Fe01 N1 91.73(6) . 2_666 ?
N5 Fe01 N1 88.27(6) . . ?
N5 Fe01 N1 88.27(6) 2_666 2_666 ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 92.00(6) 2_666 . ?
N3 Fe01 N1 88.00(6) . . ?
N3 Fe01 N1 92.00(6) . 2_666 ?
N3 Fe01 N1 88.00(6) 2_666 2_666 ?
N3 Fe01 N5 90.30(6) . . ?
N3 Fe01 N5 90.30(6) 2_666 2_666 ?
N3 Fe01 N5 89.70(6) 2_666 . ?
N3 Fe01 N5 89.70(6) . 2_666 ?
N3 Fe01 N3 180.0 2_666 . ?
N7 Fe02 N7 180.0 2_777 . ?
N11 Fe02 N7 92.12(6) . 2_777 ?
N11 Fe02 N7 87.88(6) 2_777 2_777 ?
N11 Fe02 N7 92.12(6) 2_777 . ?
N11 Fe02 N7 87.88(6) . . ?
N11 Fe02 N11 180.0 . 2_777 ?
N9 Fe02 N7 88.01(6) . . ?
N9 Fe02 N7 91.99(6) . 2_777 ?
N9 Fe02 N7 91.99(6) 2_777 . ?
N9 Fe02 N7 88.01(6) 2_777 2_777 ?
N9 Fe02 N11 89.60(6) . 2_777 ?
N9 Fe02 N11 90.40(6) 2_777 2_777 ?
N9 Fe02 N11 89.60(6) 2_777 . ?
N9 Fe02 N11 90.40(6) . . ?
N9 Fe02 N9 180.0 2_777 . ?
N8 N7 Fe02 118.09(11) . . ?
C12 N7 Fe02 135.28(13) . . ?
C12 N7 N8 106.62(14) . . ?
N1 N2 B1 118.76(13) . . ?
C3 N2 N1 110.18(14) . . ?
C3 N2 B1 130.99(15) . . ?
N9 N10 B2 118.32(14) . . ?
C17 N10 N9 109.56(15) . . ?
C17 N10 B2 132.10(15) . . ?
N7 N8 B2 118.53(14) . . ?
C14 N8 N7 109.81(15) . . ?
C14 N8 B2 131.65(16) . . ?
N2 N1 Fe01 117.64(10) . . ?
C1 N1 Fe01 135.81(12) . . ?
C1 N1 N2 106.33(14) . . ?
N12 N11 Fe02 119.48(11) . . ?
C18 N11 Fe02 133.85(13) . . ?
C18 N11 N12 106.52(14) . . ?
N5 N6 B1 118.02(13) . . ?
C9 N6 N5 109.63(16) . . ?
C9 N6 B1 132.04(16) . . ?
N6 N5 Fe01 119.64(11) . . ?
C7 N5 Fe01 133.64(13) . . ?
C7 N5 N6 106.62(15) . . ?
N3 N4 B1 119.06(14) . . ?
C6 N4 N3 109.69(15) . . ?
C6 N4 B1 131.24(16) . . ?
N11 N12 B2 117.98(13) . . ?
C20 N12 N11 109.57(15) . . ?
C20 N12 B2 132.42(15) . . ?
N10 N9 Fe02 119.30(11) . . ?
C15 N9 Fe02 134.15(13) . . ?
C15 N9 N10 106.47(15) . . ?
N4 N3 Fe01 118.84(11) . . ?
C4 N3 Fe01 134.69(13) . . ?
C4 N3 N4 106.42(15) . . ?
N8 C14 C13 107.49(17) . . ?
N8 C14 C22 122.96(19) . . ?
C13 C14 C22 129.55(18) . . ?
C14 C13 H13 126.7 . . ?
C14 C13 C12 106.64(16) . . ?
C12 C13 H13 126.7 . . ?
N7 C12 C13 109.43(17) . . ?
N7 C12 C21 123.49(18) . . ?
C13 C12 C21 127.08(18) . . ?
N3 C4 H4 124.7 . . ?
N3 C4 C5 110.57(18) . . ?
C5 C4 H4 124.7 . . ?
N4 C6 H6 125.9 . . ?
N4 C6 C5 108.29(17) . . ?
C5 C6 H6 125.9 . . ?
N10 C17 H17 125.5 . . ?
N10 C17 C16 108.93(17) . . ?
C16 C17 H17 125.5 . . ?
C4 C5 H5 127.5 . . ?
C6 C5 C4 105.02(18) . . ?
C6 C5 H5 127.5 . . ?
N2 C3 C2 107.27(15) . . ?
N2 C3 C11 122.48(17) . . ?
C2 C3 C11 130.24(17) . . ?
N9 C15 H15 124.7 . . ?
N9 C15 C16 110.56(17) . . ?
C16 C15 H15 124.7 . . ?
N1 C1 C2 109.54(16) . . ?
N1 C1 C10 123.91(17) . . ?
C2 C1 C10 126.55(18) . . ?
C3 C2 C1 106.66(16) . . ?
C3 C2 H2 126.7 . . ?
C1 C2 H2 126.7 . . ?
C17 C16 C15 104.47(17) . . ?
C17 C16 H16 127.8 . . ?
C15 C16 H16 127.8 . . ?
N11 C18 H18 124.8 . . ?
N11 C18 C19 110.37(18) . . ?
C19 C18 H18 124.8 . . ?
N5 C7 H7 124.9 . . ?
N5 C7 C8 110.29(18) . . ?
C8 C7 H7 124.9 . . ?
N12 C20 H20 125.8 . . ?
N12 C20 C19 108.33(17) . . ?
C19 C20 H20 125.8 . . ?
N6 C9 H9 125.8 . . ?
N6 C9 C8 108.47(17) . . ?
C8 C9 H9 125.8 . . ?
C18 C19 H19 127.4 . . ?
C20 C19 C18 105.20(17) . . ?
C20 C19 H19 127.4 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.5 . . ?
C9 C8 C7 104.99(18) . . ?
C9 C8 H8 127.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 106.50(15) . . ?
N2 B1 H1 111.7(11) . . ?
N6 B1 H1 108.3(11) . . ?
N4 B1 N2 108.56(14) . . ?
N4 B1 N6 107.61(14) . . ?
N4 B1 H1 113.9(10) . . ?
N10 B2 H2A 109.3(11) . . ?
N8 B2 N10 107.97(14) . . ?
N8 B2 N12 108.05(15) . . ?
N8 B2 H2A 113.0(11) . . ?
N12 B2 N10 107.14(15) . . ?
N12 B2 H2A 111.1(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -173.33(13) . . . . ?
Fe01 N1 C1 C10 6.7(3) . . . . ?
Fe01 N5 C7 C8 175.35(14) . . . . ?
Fe01 N3 C4 C5 176.65(15) . . . . ?
Fe02 N7 N8 C14 -178.20(12) . . . . ?
Fe02 N7 N8 B2 0.8(2) . . . . ?
Fe02 N7 C12 C13 177.75(14) . . . . ?
Fe02 N7 C12 C21 -2.5(3) . . . . ?
Fe02 N11 N12 C20 175.39(12) . . . . ?
Fe02 N11 N12 B2 -2.9(2) . . . . ?
Fe02 N11 C18 C19 -174.72(13) . . . . ?
Fe02 N9 C15 C16 176.15(14) . . . . ?
N7 N8 C14 C13 -0.2(2) . . . . ?
N7 N8 C14 C22 179.92(17) . . . . ?
N7 N8 B2 N10 -58.1(2) . . . . ?
N7 N8 B2 N12 57.49(19) . . . . ?
N2 N1 C1 C2 0.9(2) . . . . ?
N2 N1 C1 C10 -179.06(17) . . . . ?
N2 C3 C2 C1 -0.7(2) . . . . ?
N10 N9 C15 C16 -0.4(2) . . . . ?
N10 C17 C16 C15 0.2(2) . . . . ?
N8 N7 C12 C13 -0.7(2) . . . . ?
N8 N7 C12 C21 179.01(19) . . . . ?
N8 C14 C13 C12 -0.2(2) . . . . ?
N1 N2 C3 C2 1.25(19) . . . . ?
N1 N2 C3 C11 -177.73(16) . . . . ?
N1 N2 B1 N6 60.70(19) . . . . ?
N1 N2 B1 N4 -54.9(2) . . . . ?
N1 C1 C2 C3 -0.1(2) . . . . ?
N11 N12 C20 C19 0.6(2) . . . . ?
N11 N12 B2 N10 59.49(19) . . . . ?
N11 N12 B2 N8 -56.62(19) . . . . ?
N11 C18 C19 C20 -0.4(2) . . . . ?
N6 N5 C7 C8 -0.8(2) . . . . ?
N6 C9 C8 C7 0.1(2) . . . . ?
N5 N6 C9 C8 -0.6(2) . . . . ?
N5 N6 B1 N2 -58.32(19) . . . . ?
N5 N6 B1 N4 57.94(19) . . . . ?
N5 C7 C8 C9 0.5(2) . . . . ?
N4 N3 C4 C5 -0.6(2) . . . . ?
N4 C6 C5 C4 0.2(2) . . . . ?
N12 N11 C18 C19 0.7(2) . . . . ?
N12 C20 C19 C18 -0.2(2) . . . . ?
N9 N10 C17 C16 -0.5(2) . . . . ?
N9 N10 B2 N8 55.4(2) . . . . ?
N9 N10 B2 N12 -60.78(19) . . . . ?
N9 C15 C16 C17 0.1(2) . . . . ?
N3 N4 C6 C5 -0.6(2) . . . . ?
N3 N4 B1 N2 55.2(2) . . . . ?
N3 N4 B1 N6 -59.71(19) . . . . ?
N3 C4 C5 C6 0.3(3) . . . . ?
C14 N8 B2 N10 120.67(19) . . . . ?
C14 N8 B2 N12 -123.77(19) . . . . ?
C14 C13 C12 N7 0.6(2) . . . . ?
C14 C13 C12 C21 -179.1(2) . . . . ?
C12 N7 N8 C14 0.6(2) . . . . ?
C12 N7 N8 B2 179.59(15) . . . . ?
C6 N4 N3 Fe01 -177.03(13) . . . . ?
C6 N4 N3 C4 0.8(2) . . . . ?
C6 N4 B1 N2 -123.7(2) . . . . ?
C6 N4 B1 N6 121.4(2) . . . . ?
C17 N10 N9 Fe02 -176.62(13) . . . . ?
C17 N10 N9 C15 0.6(2) . . . . ?
C17 N10 B2 N8 -122.9(2) . . . . ?
C17 N10 B2 N12 120.9(2) . . . . ?
C3 N2 N1 Fe01 174.11(11) . . . . ?
C3 N2 N1 C1 -1.33(19) . . . . ?
C3 N2 B1 N6 -115.72(19) . . . . ?
C3 N2 B1 N4 128.66(18) . . . . ?
C18 N11 N12 C20 -0.8(2) . . . . ?
C18 N11 N12 B2 -179.19(15) . . . . ?
C20 N12 B2 N10 -118.4(2) . . . . ?
C20 N12 B2 N8 125.51(19) . . . . ?
C9 N6 N5 Fe01 -175.94(12) . . . . ?
C9 N6 N5 C7 0.9(2) . . . . ?
C9 N6 B1 N2 114.5(2) . . . . ?
C9 N6 B1 N4 -129.21(19) . . . . ?
C22 C14 C13 C12 179.6(2) . . . . ?
C10 C1 C2 C3 179.80(19) . . . . ?
C11 C3 C2 C1 178.19(19) . . . . ?
B1 N2 N1 Fe01 -3.01(19) . . . . ?
B1 N2 N1 C1 -178.45(15) . . . . ?
B1 N2 C3 C2 177.92(18) . . . . ?
B1 N2 C3 C11 -1.1(3) . . . . ?
B1 N6 N5 Fe01 -1.6(2) . . . . ?
B1 N6 N5 C7 175.24(16) . . . . ?
B1 N6 C9 C8 -173.90(19) . . . . ?
B1 N4 N3 Fe01 3.9(2) . . . . ?
B1 N4 N3 C4 -178.31(16) . . . . ?
B1 N4 C6 C5 178.32(19) . . . . ?
B2 N10 N9 Fe02 4.7(2) . . . . ?
B2 N10 N9 C15 -178.09(16) . . . . ?
B2 N10 C17 C16 177.93(19) . . . . ?
B2 N8 C14 C13 -179.03(18) . . . . ?
B2 N8 C14 C22 1.1(3) . . . . ?
B2 N12 C20 C19 178.64(18) . . . . ?


_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_250K
_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_pr210_300kdown
_database_code_depnum_ccdc_archive 'CCDC 2261112'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8669(4)
_cell_length_b                   10.7177(4)
_cell_length_c                   12.2314(5)
_cell_angle_alpha                93.061(3)
_cell_angle_beta                 94.938(3)
_cell_angle_gamma                95.503(2)
_cell_volume                     1280.25(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5702
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.788
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10936
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         3.251
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered afull sphere of reciprocal space by a combination of 7 sets of ω scans each set at different φ and/or
 2θ angles and each scan (240.00 s exposure) covering 2.000\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4700
_reflns_number_total             5815
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.053
_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)+(0.0619P)²+0.2707P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.04207(11) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.04267(11) Uani 1 2 d S . P . .
N7 N 0.80906(16) 1.00934(15) 0.92631(14) 0.0521(4) Uani 1 1 d . . . . .
N2 N 0.78088(15) 0.55331(15) 0.43808(13) 0.0490(3) Uani 1 1 d . . . . .
N10 N 0.86374(16) 0.74573(15) 0.96504(14) 0.0515(4) Uani 1 1 d . . . . .
N8 N 0.70897(15) 0.91468(16) 0.94228(14) 0.0512(4) Uani 1 1 d . . . . .
N1 N 0.69397(16) 0.58801(15) 0.51455(13) 0.0487(3) Uani 1 1 d . . . . .
N11 N 0.91202(16) 0.95668(15) 1.13624(13) 0.0510(4) Uani 1 1 d . . . . .
N6 N 0.60484(17) 0.48992(16) 0.28334(13) 0.0522(4) Uani 1 1 d . . . . .
N5 N 0.49578(16) 0.51869(16) 0.33723(13) 0.0515(4) Uani 1 1 d . . . . .
N4 N 0.68001(16) 0.32954(15) 0.40928(14) 0.0525(4) Uani 1 1 d . . . . .
N12 N 0.80294(16) 0.86770(15) 1.12931(14) 0.0511(4) Uani 1 1 d . . . . .
N9 N 0.98035(16) 0.81848(15) 0.94897(14) 0.0518(4) Uani 1 1 d . . . . .
N3 N 0.58289(17) 0.33823(15) 0.48160(13) 0.0519(4) Uani 1 1 d . . . . .
C14 C 0.5897(2) 0.9348(2) 0.88541(17) 0.0593(5) Uani 1 1 d . . . . .
C13 C 0.6135(2) 1.0429(3) 0.83294(19) 0.0686(6) Uani 1 1 d . . . . .
H13 H 0.550399 1.079839 0.787454 0.082 Uiso 1 1 calc R U . . .
C12 C 0.7500(2) 1.0876(2) 0.86032(18) 0.0605(5) Uani 1 1 d . . . . .
C4 C 0.5619(2) 0.2250(2) 0.5209(2) 0.0646(5) Uani 1 1 d . . . . .
H4 H 0.500756 0.204083 0.572415 0.078 Uiso 1 1 calc R U . . .
C6 C 0.7164(2) 0.2115(2) 0.4038(2) 0.0651(5) Uani 1 1 d . . . . .
H6 H 0.779928 0.181873 0.359594 0.078 Uiso 1 1 calc R U . . .
C17 C 0.8740(2) 0.6266(2) 0.92992(19) 0.0638(5) Uani 1 1 d . . . . .
H17 H 0.807498 0.559420 0.932589 0.077 Uiso 1 1 calc R U . . .
C5 C 0.6440(3) 0.1428(2) 0.4741(2) 0.0755(7) Uani 1 1 d . . . . .
H5 H 0.648854 0.058763 0.487795 0.091 Uiso 1 1 calc R U . . .
C3 C 0.90000(19) 0.62764(19) 0.45252(17) 0.0522(4) Uani 1 1 d . . . . .
C15 C 1.0614(2) 0.7425(2) 0.90288(19) 0.0633(5) Uani 1 1 d . . . . .
H15 H 1.148018 0.767771 0.882522 0.076 Uiso 1 1 calc R U . . .
C1 C 0.7623(2) 0.68348(19) 0.57720(16) 0.0535(4) Uani 1 1 d . . . . .
C2 C 0.8914(2) 0.7106(2) 0.54032(18) 0.0599(5) Uani 1 1 d . . . . .
H2 H 0.958650 0.773020 0.569714 0.072 Uiso 1 1 calc R U . . .
C16 C 0.9987(3) 0.6201(2) 0.8894(2) 0.0716(6) Uani 1 1 d . . . . .
H16 H 1.033607 0.549550 0.859596 0.086 Uiso 1 1 calc R U . . .
C18 C 0.9408(2) 0.9907(2) 1.24254(18) 0.0617(5) Uani 1 1 d . . . . .
H18 H 1.010498 1.051341 1.271061 0.074 Uiso 1 1 calc R U . . .
C7 C 0.4082(2) 0.5617(2) 0.26341(19) 0.0630(5) Uani 1 1 d . . . . .
H7 H 0.323819 0.587347 0.277877 0.076 Uiso 1 1 calc R U . . .
C20 C 0.7666(2) 0.8460(2) 1.23087(18) 0.0608(5) Uani 1 1 d . . . . .
H20 H 0.695674 0.788785 1.247747 0.073 Uiso 1 1 calc R U . . .
C9 C 0.5842(3) 0.5172(2) 0.17736(17) 0.0660(6) Uani 1 1 d . . . . .
H9 H 0.644384 0.506635 0.123874 0.079 Uiso 1 1 calc R U . . .
C19 C 0.8524(3) 0.9230(2) 1.30463(19) 0.0704(6) Uani 1 1 d . . . . .
H19 H 0.851492 0.928800 1.380698 0.085 Uiso 1 1 calc R U . . .
C21 C 0.8239(3) 1.2039(3) 0.8251(3) 0.0841(8) Uani 1 1 d . . . . .
H21A H 0.794117 1.275719 0.862944 0.126 Uiso 1 1 calc R U . . .
H21B H 0.804762 1.208860 0.747284 0.126 Uiso 1 1 calc R U . . .
H21C H 0.920407 1.202197 0.842438 0.126 Uiso 1 1 calc R U . . .
C8 C 0.4602(3) 0.5629(3) 0.1618(2) 0.0736(6) Uani 1 1 d . . . . .
H8 H 0.419234 0.589245 0.096819 0.088 Uiso 1 1 calc R U . . .
C22 C 0.4612(2) 0.8483(3) 0.8856(2) 0.0819(7) Uani 1 1 d . . . . .
H22A H 0.473885 0.767980 0.851608 0.123 Uiso 1 1 calc R U . . .
H22B H 0.387382 0.883105 0.845352 0.123 Uiso 1 1 calc R U . . .
H22C H 0.439932 0.838449 0.959974 0.123 Uiso 1 1 calc R U . . .
C10 C 0.7059(3) 0.7481(2) 0.6716(2) 0.0698(6) Uani 1 1 d . . . . .
H10A H 0.691754 0.832534 0.654521 0.105 Uiso 1 1 calc R U . . .
H10B H 0.769257 0.749681 0.735897 0.105 Uiso 1 1 calc R U . . .
H10C H 0.620393 0.703667 0.685129 0.105 Uiso 1 1 calc R U . . .
C11 C 1.0135(2) 0.6160(2) 0.3797(2) 0.0668(6) Uani 1 1 d . . . . .
H11A H 1.037986 0.531378 0.378033 0.100 Uiso 1 1 calc R U . . .
H11B H 1.091499 0.672594 0.407927 0.100 Uiso 1 1 calc R U . . .
H11C H 0.983728 0.636479 0.306670 0.100 Uiso 1 1 calc R U . . .
B1 B 0.7296(2) 0.4467(2) 0.35101(19) 0.0522(5) Uani 1 1 d . . . . .
B2 B 0.7466(2) 0.8085(2) 1.01443(19) 0.0513(5) Uani 1 1 d . . . . .
H1 H 0.808(2) 0.4294(19) 0.2965(17) 0.051(5) Uiso 1 1 d . . . . .
H2A H 0.659(2) 0.735(2) 1.0214(19) 0.061(6) Uiso 1 1 d . . . . .


_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 2.0400(16) 2_666 ?
Fe01 N1 2.0400(16) . ?
Fe01 N5 2.0089(16) 2_666 ?
Fe01 N5 2.0088(16) . ?
Fe01 N3 1.9969(16) . ?
Fe01 N3 1.9969(16) 2_666 ?
Fe02 N7 2.0311(16) 2_777 ?
Fe02 N7 2.0310(16) . ?
Fe02 N11 2.0001(16) . ?
Fe02 N11 2.0001(16) 2_777 ?
Fe02 N9 1.9973(17) 2_777 ?
Fe02 N9 1.9973(17) . ?
N7 N8 1.380(2) . ?
N7 C12 1.334(3) . ?
N2 N1 1.382(2) . ?
N2 C3 1.348(2) . ?
N2 B1 1.537(3) . ?
N10 N9 1.361(2) . ?
N10 C17 1.341(3) . ?
N10 B2 1.543(3) . ?
N8 C14 1.356(3) . ?
N8 B2 1.531(3) . ?
N1 C1 1.336(2) . ?
N11 N12 1.362(2) . ?
N11 C18 1.331(3) . ?
N6 N5 1.361(2) . ?
N6 C9 1.347(3) . ?
N6 B1 1.546(3) . ?
N5 C7 1.327(3) . ?
N4 N3 1.365(2) . ?
N4 C6 1.347(3) . ?
N4 B1 1.537(3) . ?
N12 C20 1.348(3) . ?
N12 B2 1.546(3) . ?
N9 C15 1.332(3) . ?
N3 C4 1.334(3) . ?
C14 C13 1.365(3) . ?
C14 C22 1.497(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.392(3) . ?
C12 C21 1.485(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.387(3) . ?
C6 H6 0.9300 . ?
C6 C5 1.365(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.372(3) . ?
C5 H5 0.9300 . ?
C3 C2 1.371(3) . ?
C3 C11 1.500(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.391(3) . ?
C1 C2 1.397(3) . ?
C1 C10 1.490(3) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.384(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.385(3) . ?
C20 H20 0.9300 . ?
C20 C19 1.366(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.363(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.09(2) . ?
B2 H2A 1.12(2) . ?

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 180.0 . 2_666 ?
N5 Fe01 N1 87.92(6) . . ?
N5 Fe01 N1 92.08(6) 2_666 . ?
N5 Fe01 N1 92.08(6) . 2_666 ?
N5 Fe01 N1 87.92(6) 2_666 2_666 ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 87.38(6) 2_666 2_666 ?
N3 Fe01 N1 87.38(6) . . ?
N3 Fe01 N1 92.62(6) 2_666 . ?
N3 Fe01 N1 92.62(6) . 2_666 ?
N3 Fe01 N5 90.02(7) 2_666 . ?
N3 Fe01 N5 89.98(7) 2_666 2_666 ?
N3 Fe01 N5 90.02(7) . 2_666 ?
N3 Fe01 N5 89.98(7) . . ?
N3 Fe01 N3 180.00(9) . 2_666 ?
N7 Fe02 N7 180.0 . 2_777 ?
N11 Fe02 N7 87.42(7) 2_777 2_777 ?
N11 Fe02 N7 92.58(6) . 2_777 ?
N11 Fe02 N7 87.42(7) . . ?
N11 Fe02 N7 92.58(6) 2_777 . ?
N11 Fe02 N11 180.00(9) 2_777 . ?
N9 Fe02 N7 87.50(7) . . ?
N9 Fe02 N7 92.50(7) . 2_777 ?
N9 Fe02 N7 92.50(7) 2_777 . ?
N9 Fe02 N7 87.50(7) 2_777 2_777 ?
N9 Fe02 N11 90.00(7) 2_777 . ?
N9 Fe02 N11 90.00(7) . . ?
N9 Fe02 N11 90.00(7) . 2_777 ?
N9 Fe02 N11 90.00(7) 2_777 2_777 ?
N9 Fe02 N9 180.0 . 2_777 ?
N8 N7 Fe02 117.96(12) . . ?
C12 N7 Fe02 135.56(15) . . ?
C12 N7 N8 106.46(16) . . ?
N1 N2 B1 118.77(14) . . ?
C3 N2 N1 110.35(15) . . ?
C3 N2 B1 130.82(16) . . ?
N9 N10 B2 118.74(15) . . ?
C17 N10 N9 109.61(17) . . ?
C17 N10 B2 131.63(17) . . ?
N7 N8 B2 118.78(15) . . ?
C14 N8 N7 109.81(17) . . ?
C14 N8 B2 131.40(18) . . ?
N2 N1 Fe01 117.60(11) . . ?
C1 N1 Fe01 135.96(13) . . ?
C1 N1 N2 106.19(15) . . ?
N12 N11 Fe02 119.46(12) . . ?
C18 N11 Fe02 134.02(15) . . ?
C18 N11 N12 106.36(17) . . ?
N5 N6 B1 118.28(15) . . ?
C9 N6 N5 109.33(18) . . ?
C9 N6 B1 132.09(18) . . ?
N6 N5 Fe01 119.36(12) . . ?
C7 N5 Fe01 134.01(15) . . ?
C7 N5 N6 106.53(17) . . ?
N3 N4 B1 119.18(15) . . ?
C6 N4 N3 109.47(17) . . ?
C6 N4 B1 131.35(18) . . ?
N11 N12 B2 118.31(15) . . ?
C20 N12 N11 109.74(18) . . ?
C20 N12 B2 131.92(18) . . ?
N10 N9 Fe02 119.14(12) . . ?
C15 N9 Fe02 134.45(15) . . ?
C15 N9 N10 106.34(17) . . ?
N4 N3 Fe01 118.69(12) . . ?
C4 N3 Fe01 134.88(15) . . ?
C4 N3 N4 106.33(17) . . ?
N8 C14 C13 107.12(19) . . ?
N8 C14 C22 122.9(2) . . ?
C13 C14 C22 130.0(2) . . ?
C14 C13 H13 126.4 . . ?
C14 C13 C12 107.12(19) . . ?
C12 C13 H13 126.4 . . ?
N7 C12 C13 109.5(2) . . ?
N7 C12 C21 123.1(2) . . ?
C13 C12 C21 127.4(2) . . ?
N3 C4 H4 124.8 . . ?
N3 C4 C5 110.4(2) . . ?
C5 C4 H4 124.8 . . ?
N4 C6 H6 125.8 . . ?
N4 C6 C5 108.4(2) . . ?
C5 C6 H6 125.8 . . ?
N10 C17 H17 125.6 . . ?
N10 C17 C16 108.75(19) . . ?
C16 C17 H17 125.6 . . ?
C4 C5 H5 127.3 . . ?
C6 C5 C4 105.4(2) . . ?
C6 C5 H5 127.3 . . ?
N2 C3 C2 107.10(17) . . ?
N2 C3 C11 122.97(19) . . ?
C2 C3 C11 129.92(19) . . ?
N9 C15 H15 124.7 . . ?
N9 C15 C16 110.7(2) . . ?
C16 C15 H15 124.7 . . ?
N1 C1 C2 109.47(18) . . ?
N1 C1 C10 123.75(19) . . ?
C2 C1 C10 126.78(19) . . ?
C3 C2 C1 106.89(18) . . ?
C3 C2 H2 126.6 . . ?
C1 C2 H2 126.6 . . ?
C17 C16 C15 104.6(2) . . ?
C17 C16 H16 127.7 . . ?
C15 C16 H16 127.7 . . ?
N11 C18 H18 124.8 . . ?
N11 C18 C19 110.3(2) . . ?
C19 C18 H18 124.8 . . ?
N5 C7 H7 124.8 . . ?
N5 C7 C8 110.5(2) . . ?
C8 C7 H7 124.8 . . ?
N12 C20 H20 126.0 . . ?
N12 C20 C19 107.9(2) . . ?
C19 C20 H20 126.0 . . ?
N6 C9 H9 125.8 . . ?
N6 C9 C8 108.4(2) . . ?
C8 C9 H9 125.8 . . ?
C18 C19 H19 127.2 . . ?
C20 C19 C18 105.7(2) . . ?
C20 C19 H19 127.2 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.4 . . ?
C9 C8 C7 105.2(2) . . ?
C9 C8 H8 127.4 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 106.88(16) . . ?
N2 B1 H1 110.9(11) . . ?
N6 B1 H1 109.1(11) . . ?
N4 B1 N2 108.95(16) . . ?
N4 B1 N6 107.86(16) . . ?
N4 B1 H1 112.9(11) . . ?
N10 B2 N12 107.25(16) . . ?
N10 B2 H2A 109.1(12) . . ?
N8 B2 N10 108.20(16) . . ?
N8 B2 N12 107.98(16) . . ?
N8 B2 H2A 113.6(12) . . ?
N12 B2 H2A 110.5(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -173.18(15) . . . . ?
Fe01 N1 C1 C10 7.1(3) . . . . ?
Fe01 N5 C7 C8 175.24(16) . . . . ?
Fe01 N3 C4 C5 175.80(17) . . . . ?
Fe02 N7 N8 C14 -178.68(13) . . . . ?
Fe02 N7 N8 B2 0.2(2) . . . . ?
Fe02 N7 C12 C13 178.25(16) . . . . ?
Fe02 N7 C12 C21 -2.3(4) . . . . ?
Fe02 N11 N12 C20 175.15(13) . . . . ?
Fe02 N11 N12 B2 -3.2(2) . . . . ?
Fe02 N11 C18 C19 -174.40(15) . . . . ?
Fe02 N9 C15 C16 176.51(17) . . . . ?
N7 N8 C14 C13 -0.1(2) . . . . ?
N7 N8 C14 C22 179.9(2) . . . . ?
N7 N8 B2 N10 -57.8(2) . . . . ?
N7 N8 B2 N12 58.0(2) . . . . ?
N2 N1 C1 C2 0.7(2) . . . . ?
N2 N1 C1 C10 -179.06(19) . . . . ?
N2 C3 C2 C1 -0.4(2) . . . . ?
N10 N9 C15 C16 -0.4(3) . . . . ?
N10 C17 C16 C15 0.1(3) . . . . ?
N8 N7 C12 C13 -0.7(2) . . . . ?
N8 N7 C12 C21 178.8(2) . . . . ?
N8 C14 C13 C12 -0.3(3) . . . . ?
N1 N2 C3 C2 0.8(2) . . . . ?
N1 N2 C3 C11 -177.94(18) . . . . ?
N1 N2 B1 N6 61.1(2) . . . . ?
N1 N2 B1 N4 -55.2(2) . . . . ?
N1 C1 C2 C3 -0.2(2) . . . . ?
N11 N12 C20 C19 0.7(2) . . . . ?
N11 N12 B2 N10 59.7(2) . . . . ?
N11 N12 B2 N8 -56.7(2) . . . . ?
N11 C18 C19 C20 -0.5(3) . . . . ?
N6 N5 C7 C8 -0.8(2) . . . . ?
N6 C9 C8 C7 0.1(3) . . . . ?
N5 N6 C9 C8 -0.6(2) . . . . ?
N5 N6 B1 N2 -58.8(2) . . . . ?
N5 N6 B1 N4 58.2(2) . . . . ?
N5 C7 C8 C9 0.5(3) . . . . ?
N4 N3 C4 C5 -0.4(3) . . . . ?
N4 C6 C5 C4 0.6(3) . . . . ?
N12 N11 C18 C19 0.9(2) . . . . ?
N12 C20 C19 C18 -0.1(3) . . . . ?
N9 N10 C17 C16 -0.3(3) . . . . ?
N9 N10 B2 N8 55.7(2) . . . . ?
N9 N10 B2 N12 -60.6(2) . . . . ?
N9 C15 C16 C17 0.2(3) . . . . ?
N3 N4 C6 C5 -0.9(3) . . . . ?
N3 N4 B1 N2 55.3(2) . . . . ?
N3 N4 B1 N6 -60.4(2) . . . . ?
N3 C4 C5 C6 -0.2(3) . . . . ?
C14 N8 B2 N10 120.8(2) . . . . ?
C14 N8 B2 N12 -123.4(2) . . . . ?
C14 C13 C12 N7 0.7(3) . . . . ?
C14 C13 C12 C21 -178.8(2) . . . . ?
C12 N7 N8 C14 0.5(2) . . . . ?
C12 N7 N8 B2 179.34(18) . . . . ?
C6 N4 N3 Fe01 -176.15(14) . . . . ?
C6 N4 N3 C4 0.7(2) . . . . ?
C6 N4 B1 N2 -124.0(2) . . . . ?
C6 N4 B1 N6 120.3(2) . . . . ?
C17 N10 N9 Fe02 -177.03(14) . . . . ?
C17 N10 N9 C15 0.4(2) . . . . ?
C17 N10 B2 N8 -122.5(2) . . . . ?
C17 N10 B2 N12 121.3(2) . . . . ?
C3 N2 N1 Fe01 174.25(12) . . . . ?
C3 N2 N1 C1 -0.9(2) . . . . ?
C3 N2 B1 N6 -115.7(2) . . . . ?
C3 N2 B1 N4 128.0(2) . . . . ?
C18 N11 N12 C20 -0.9(2) . . . . ?
C18 N11 N12 B2 -179.29(17) . . . . ?
C20 N12 B2 N10 -118.2(2) . . . . ?
C20 N12 B2 N8 125.4(2) . . . . ?
C9 N6 N5 Fe01 -175.88(14) . . . . ?
C9 N6 N5 C7 0.9(2) . . . . ?
C9 N6 B1 N2 114.1(2) . . . . ?
C9 N6 B1 N4 -128.8(2) . . . . ?
C22 C14 C13 C12 179.7(2) . . . . ?
C10 C1 C2 C3 179.5(2) . . . . ?
C11 C3 C2 C1 178.3(2) . . . . ?
B1 N2 N1 Fe01 -3.2(2) . . . . ?
B1 N2 N1 C1 -178.33(17) . . . . ?
B1 N2 C3 C2 177.8(2) . . . . ?
B1 N2 C3 C11 -1.0(3) . . . . ?
B1 N6 N5 Fe01 -1.4(2) . . . . ?
B1 N6 N5 C7 175.37(17) . . . . ?
B1 N6 C9 C8 -174.0(2) . . . . ?
B1 N4 N3 Fe01 4.4(2) . . . . ?
B1 N4 N3 C4 -178.73(18) . . . . ?
B1 N4 C6 C5 178.5(2) . . . . ?
B2 N10 N9 Fe02 4.5(2) . . . . ?
B2 N10 N9 C15 -178.05(18) . . . . ?
B2 N10 C17 C16 177.9(2) . . . . ?
B2 N8 C14 C13 -178.7(2) . . . . ?
B2 N8 C14 C22 1.2(3) . . . . ?
B2 N12 C20 C19 178.7(2) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_300Kdown
_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_pr210_300k
_database_code_depnum_ccdc_archive 'CCDC 2261111'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8706(5)
_cell_length_b                   10.7248(5)
_cell_length_c                   12.2325(5)
_cell_angle_alpha                93.064(4)
_cell_angle_beta                 94.942(3)
_cell_angle_gamma                95.509(3)
_cell_volume                     1281.67(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5733
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.788
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10923
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.250
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 6 sets of ω scans each set at different φ and/or 2θ angles and each scan (120.00 s exposure) covering 2.000\ degrees in ω.
The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4447
_reflns_number_total             5829
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0395
_refine_ls_restrained_S_all      1.025
_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)+(0.0683P)²+0.1572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1171
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.04318(12) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.04379(12) Uani 1 2 d S . P . .
N7 N 0.80919(17) 1.00912(16) 0.92647(14) 0.0530(4) Uani 1 1 d . . . . .
N2 N 0.78095(16) 0.55351(15) 0.43805(13) 0.0495(4) Uani 1 1 d . . . . .
N10 N 0.86373(17) 0.74598(15) 0.96505(14) 0.0527(4) Uani 1 1 d . . . . .
N8 N 0.70874(16) 0.91466(16) 0.94230(14) 0.0520(4) Uani 1 1 d . . . . .
N1 N 0.69367(16) 0.58795(15) 0.51415(13) 0.0495(4) Uani 1 1 d . . . . .
N11 N 0.91217(18) 0.95680(16) 1.13634(14) 0.0529(4) Uani 1 1 d . . . . .
N6 N 0.60462(18) 0.49015(16) 0.28335(13) 0.0533(4) Uani 1 1 d . . . . .
N5 N 0.49596(17) 0.51864(16) 0.33735(14) 0.0524(4) Uani 1 1 d . . . . .
N4 N 0.67984(17) 0.32959(16) 0.40943(14) 0.0535(4) Uani 1 1 d . . . . .
N12 N 0.80275(17) 0.86748(16) 1.12915(14) 0.0523(4) Uani 1 1 d . . . . .
N9 N 0.98052(17) 0.81850(16) 0.94889(14) 0.0528(4) Uani 1 1 d . . . . .
N3 N 0.58282(18) 0.33824(16) 0.48149(14) 0.0532(4) Uani 1 1 d . . . . .
C14 C 0.5897(2) 0.9350(2) 0.88549(18) 0.0610(5) Uani 1 1 d . . . . .
C13 C 0.6134(2) 1.0426(3) 0.8327(2) 0.0700(6) Uani 1 1 d . . . . .
H13 H 0.550368 1.079207 0.786907 0.084 Uiso 1 1 calc R U . . .
C12 C 0.7500(2) 1.0876(2) 0.86040(19) 0.0621(5) Uani 1 1 d . . . . .
C4 C 0.5623(3) 0.2252(2) 0.5208(2) 0.0648(6) Uani 1 1 d . . . . .
H4 H 0.501393 0.204420 0.572489 0.078 Uiso 1 1 calc R U . . .
C6 C 0.7165(2) 0.2116(2) 0.4040(2) 0.0671(6) Uani 1 1 d . . . . .
H6 H 0.780204 0.182022 0.359924 0.080 Uiso 1 1 calc R U . . .
C17 C 0.8743(3) 0.6267(2) 0.9300(2) 0.0649(6) Uani 1 1 d . . . . .
H17 H 0.807981 0.559533 0.932726 0.078 Uiso 1 1 calc R U . . .
C5 C 0.6437(3) 0.1428(2) 0.4743(2) 0.0759(7) Uani 1 1 d . . . . .
H5 H 0.648181 0.058785 0.487965 0.091 Uiso 1 1 calc R U . . .
C3 C 0.8999(2) 0.6277(2) 0.45261(17) 0.0541(5) Uani 1 1 d . . . . .
C15 C 1.0612(2) 0.7427(2) 0.9029(2) 0.0654(6) Uani 1 1 d . . . . .
H15 H 1.147632 0.768089 0.882366 0.078 Uiso 1 1 calc R U . . .
C1 C 0.7625(2) 0.68362(19) 0.57734(17) 0.0548(5) Uani 1 1 d . . . . .
C2 C 0.8913(2) 0.7106(2) 0.54034(19) 0.0608(5) Uani 1 1 d . . . . .
H2 H 0.958560 0.772943 0.569670 0.073 Uiso 1 1 calc R U . . .
C16 C 0.9989(3) 0.6203(2) 0.8896(2) 0.0730(6) Uani 1 1 d . . . . .
H16 H 1.033980 0.549832 0.859983 0.088 Uiso 1 1 calc R U . . .
C18 C 0.9407(3) 0.9905(2) 1.24257(19) 0.0631(5) Uani 1 1 d . . . . .
H18 H 1.010437 1.050924 1.271199 0.076 Uiso 1 1 calc R U . . .
C7 C 0.4083(2) 0.5617(2) 0.26365(19) 0.0644(6) Uani 1 1 d . . . . .
H7 H 0.323902 0.587247 0.278221 0.077 Uiso 1 1 calc R U . . .
C20 C 0.7666(3) 0.8460(2) 1.23076(19) 0.0626(5) Uani 1 1 d . . . . .
H20 H 0.695772 0.788709 1.247657 0.075 Uiso 1 1 calc R U . . .
C9 C 0.5841(3) 0.5174(2) 0.17743(18) 0.0670(6) Uani 1 1 d . . . . .
H9 H 0.644325 0.506808 0.124010 0.080 Uiso 1 1 calc R U . . .
C19 C 0.8521(3) 0.9231(2) 1.30463(19) 0.0717(6) Uani 1 1 d . . . . .
H19 H 0.851071 0.928956 1.380674 0.086 Uiso 1 1 calc R U . . .
C21 C 0.8241(3) 1.2036(3) 0.8250(3) 0.0860(8) Uani 1 1 d . . . . .
H21A H 0.789866 1.275698 0.858581 0.129 Uiso 1 1 calc R U . . .
H21B H 0.810483 1.205338 0.746497 0.129 Uiso 1 1 calc R U . . .
H21C H 0.919961 1.204589 0.847163 0.129 Uiso 1 1 calc R U . . .
C8 C 0.4602(3) 0.5631(3) 0.1617(2) 0.0743(7) Uani 1 1 d . . . . .
H8 H 0.419304 0.589475 0.096778 0.089 Uiso 1 1 calc R U . . .
C22 C 0.4614(3) 0.8485(3) 0.8858(2) 0.0840(8) Uani 1 1 d . . . . .
H22A H 0.475529 0.767140 0.854839 0.126 Uiso 1 1 calc R U . . .
H22B H 0.388546 0.881303 0.842700 0.126 Uiso 1 1 calc R U . . .
H22C H 0.437964 0.841711 0.959890 0.126 Uiso 1 1 calc R U . . .
C10 C 0.7056(3) 0.7478(2) 0.6712(2) 0.0718(6) Uani 1 1 d . . . . .
H10A H 0.619339 0.704020 0.683706 0.108 Uiso 1 1 calc R U . . .
H10B H 0.692668 0.832602 0.654598 0.108 Uiso 1 1 calc R U . . .
H10C H 0.767889 0.748350 0.736031 0.108 Uiso 1 1 calc R U . . .
C11 C 1.0135(2) 0.6160(2) 0.3795(2) 0.0693(6) Uani 1 1 d . . . . .
H11A H 1.037736 0.531434 0.377581 0.104 Uiso 1 1 calc R U . . .
H11B H 1.091573 0.672433 0.407759 0.104 Uiso 1 1 calc R U . . .
H11C H 0.983642 0.636794 0.306556 0.104 Uiso 1 1 calc R U . . .
B1 B 0.7294(2) 0.4468(2) 0.35109(19) 0.0540(5) Uani 1 1 d . . . . .
H1 H 0.801166 0.428759 0.303726 0.065 Uiso 1 1 calc R U . . .
B2 B 0.7471(2) 0.8086(2) 1.0147(2) 0.0529(5) Uani 1 1 d . . . . .
H2A H 0.667907 0.747311 1.019648 0.064 Uiso 1 1 calc R U . . .


_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 2.0380(16) 2_666 ?
Fe01 N1 2.0380(16) . ?
Fe01 N5 2.0076(16) 2_666 ?
Fe01 N5 2.0076(16) . ?
Fe01 N3 1.9978(17) 2_666 ?
Fe01 N3 1.9978(17) . ?
Fe02 N7 2.0295(17) 2_777 ?
Fe02 N7 2.0295(17) . ?
Fe02 N11 2.0006(17) . ?
Fe02 N11 2.0006(17) 2_777 ?
Fe02 N9 1.9986(17) 2_777 ?
Fe02 N9 1.9985(17) . ?
N7 N8 1.381(2) . ?
N7 C12 1.337(3) . ?
N2 N1 1.381(2) . ?
N2 C3 1.347(3) . ?
N2 B1 1.538(3) . ?
N10 N9 1.362(2) . ?
N10 C17 1.344(3) . ?
N10 B2 1.540(3) . ?
N8 C14 1.355(3) . ?
N8 B2 1.534(3) . ?
N1 C1 1.343(3) . ?
N11 N12 1.367(2) . ?
N11 C18 1.329(3) . ?
N6 N5 1.358(2) . ?
N6 C9 1.346(3) . ?
N6 B1 1.547(3) . ?
N5 C7 1.327(3) . ?
N4 N3 1.363(2) . ?
N4 C6 1.349(3) . ?
N4 B1 1.539(3) . ?
N12 C20 1.348(3) . ?
N12 B2 1.539(3) . ?
N9 C15 1.328(3) . ?
N3 C4 1.333(3) . ?
C14 C13 1.363(3) . ?
C14 C22 1.496(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.395(3) . ?
C12 C21 1.485(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.382(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.368(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.371(3) . ?
C5 H5 0.9300 . ?
C3 C2 1.370(3) . ?
C3 C11 1.503(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(3) . ?
C1 C2 1.395(3) . ?
C1 C10 1.487(3) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.384(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.389(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.366(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.363(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 0.9800 . ?
B2 H2A 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 180.0 . 2_666 ?
N5 Fe01 N1 92.26(7) . 2_666 ?
N5 Fe01 N1 87.74(7) . . ?
N5 Fe01 N1 92.26(7) 2_666 . ?
N5 Fe01 N1 87.74(7) 2_666 2_666 ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 87.41(7) . . ?
N3 Fe01 N1 92.59(7) . 2_666 ?
N3 Fe01 N1 92.59(7) 2_666 . ?
N3 Fe01 N1 87.41(7) 2_666 2_666 ?
N3 Fe01 N5 89.91(7) . . ?
N3 Fe01 N5 90.09(7) 2_666 . ?
N3 Fe01 N5 90.09(7) . 2_666 ?
N3 Fe01 N5 89.91(7) 2_666 2_666 ?
N3 Fe01 N3 180.0 2_666 . ?
N7 Fe02 N7 180.00(4) . 2_777 ?
N11 Fe02 N7 92.60(7) 2_777 . ?
N11 Fe02 N7 87.40(7) . . ?
N11 Fe02 N7 92.60(7) . 2_777 ?
N11 Fe02 N7 87.40(7) 2_777 2_777 ?
N11 Fe02 N11 180.0 2_777 . ?
N9 Fe02 N7 87.49(7) 2_777 2_777 ?
N9 Fe02 N7 92.50(7) 2_777 . ?
N9 Fe02 N7 92.51(7) . 2_777 ?
N9 Fe02 N7 87.50(7) . . ?
N9 Fe02 N11 89.92(7) 2_777 . ?
N9 Fe02 N11 90.08(7) . . ?
N9 Fe02 N11 89.92(7) . 2_777 ?
N9 Fe02 N11 90.08(7) 2_777 2_777 ?
N9 Fe02 N9 180.00(10) . 2_777 ?
N8 N7 Fe02 118.21(12) . . ?
C12 N7 Fe02 135.48(15) . . ?
C12 N7 N8 106.30(17) . . ?
N1 N2 B1 118.43(15) . . ?
C3 N2 N1 110.52(17) . . ?
C3 N2 B1 130.98(18) . . ?
N9 N10 B2 118.82(16) . . ?
C17 N10 N9 109.37(18) . . ?
C17 N10 B2 131.80(18) . . ?
N7 N8 B2 118.34(16) . . ?
C14 N8 N7 109.89(17) . . ?
C14 N8 B2 131.76(18) . . ?
N2 N1 Fe01 117.92(12) . . ?
C1 N1 Fe01 135.90(14) . . ?
C1 N1 N2 105.97(16) . . ?
N12 N11 Fe02 119.29(13) . . ?
C18 N11 Fe02 134.24(16) . . ?
C18 N11 N12 106.31(18) . . ?
N5 N6 B1 118.12(16) . . ?
C9 N6 N5 109.53(19) . . ?
C9 N6 B1 132.06(19) . . ?
N6 N5 Fe01 119.56(13) . . ?
C7 N5 Fe01 133.86(16) . . ?
C7 N5 N6 106.47(17) . . ?
N3 N4 B1 119.15(16) . . ?
C6 N4 N3 109.55(18) . . ?
C6 N4 B1 131.29(19) . . ?
N11 N12 B2 118.28(15) . . ?
C20 N12 N11 109.52(19) . . ?
C20 N12 B2 132.17(18) . . ?
N10 N9 Fe02 118.95(13) . . ?
C15 N9 Fe02 134.56(15) . . ?
C15 N9 N10 106.42(17) . . ?
N4 N3 Fe01 118.72(12) . . ?
C4 N3 Fe01 135.01(16) . . ?
C4 N3 N4 106.18(18) . . ?
N8 C14 C13 107.3(2) . . ?
N8 C14 C22 122.7(2) . . ?
C13 C14 C22 130.0(2) . . ?
C14 C13 H13 126.5 . . ?
C14 C13 C12 107.04(19) . . ?
C12 C13 H13 126.5 . . ?
N7 C12 C13 109.5(2) . . ?
N7 C12 C21 123.0(2) . . ?
C13 C12 C21 127.5(2) . . ?
N3 C4 H4 124.6 . . ?
N3 C4 C5 110.8(2) . . ?
C5 C4 H4 124.6 . . ?
N4 C6 H6 125.9 . . ?
N4 C6 C5 108.3(2) . . ?
C5 C6 H6 125.9 . . ?
N10 C17 H17 125.6 . . ?
N10 C17 C16 108.8(2) . . ?
C16 C17 H17 125.6 . . ?
C4 C5 H5 127.4 . . ?
C6 C5 C4 105.2(2) . . ?
C6 C5 H5 127.4 . . ?
N2 C3 C2 107.12(19) . . ?
N2 C3 C11 122.9(2) . . ?
C2 C3 C11 130.0(2) . . ?
N9 C15 H15 124.6 . . ?
N9 C15 C16 110.8(2) . . ?
C16 C15 H15 124.6 . . ?
N1 C1 C2 109.36(19) . . ?
N1 C1 C10 123.5(2) . . ?
C2 C1 C10 127.2(2) . . ?
C3 C2 C1 107.01(19) . . ?
C3 C2 H2 126.5 . . ?
C1 C2 H2 126.5 . . ?
C17 C16 C15 104.5(2) . . ?
C17 C16 H16 127.7 . . ?
C15 C16 H16 127.7 . . ?
N11 C18 H18 124.8 . . ?
N11 C18 C19 110.5(2) . . ?
C19 C18 H18 124.8 . . ?
N5 C7 H7 124.8 . . ?
N5 C7 C8 110.5(2) . . ?
C8 C7 H7 124.8 . . ?
N12 C20 H20 126.0 . . ?
N12 C20 C19 108.1(2) . . ?
C19 C20 H20 126.0 . . ?
N6 C9 H9 125.8 . . ?
N6 C9 C8 108.4(2) . . ?
C8 C9 H9 125.8 . . ?
C18 C19 H19 127.2 . . ?
C20 C19 C18 105.6(2) . . ?
C20 C19 H19 127.2 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.5 . . ?
C9 C8 C7 105.1(2) . . ?
C9 C8 H8 127.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 106.88(17) . . ?
N2 B1 N4 109.04(17) . . ?
N2 B1 H1 111.0 . . ?
N6 B1 H1 111.0 . . ?
N4 B1 N6 107.92(17) . . ?
N4 B1 H1 111.0 . . ?
N10 B2 H2A 110.9 . . ?
N8 B2 N10 108.24(16) . . ?
N8 B2 N12 108.13(17) . . ?
N8 B2 H2A 110.9 . . ?
N12 B2 N10 107.57(17) . . ?
N12 B2 H2A 110.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -173.44(15) . . . . ?
Fe01 N1 C1 C10 6.5(3) . . . . ?
Fe01 N5 C7 C8 175.21(16) . . . . ?
Fe01 N3 C4 C5 175.84(18) . . . . ?
Fe02 N7 N8 C14 -178.72(14) . . . . ?
Fe02 N7 N8 B2 0.1(2) . . . . ?
Fe02 N7 C12 C13 178.10(17) . . . . ?
Fe02 N7 C12 C21 -2.0(4) . . . . ?
Fe02 N11 N12 C20 175.16(14) . . . . ?
Fe02 N11 N12 B2 -3.1(2) . . . . ?
Fe02 N11 C18 C19 -174.48(16) . . . . ?
Fe02 N9 C15 C16 176.36(17) . . . . ?
N7 N8 C14 C13 0.1(2) . . . . ?
N7 N8 C14 C22 179.8(2) . . . . ?
N7 N8 B2 N10 -57.9(2) . . . . ?
N7 N8 B2 N12 58.3(2) . . . . ?
N2 N1 C1 C2 0.9(2) . . . . ?
N2 N1 C1 C10 -179.2(2) . . . . ?
N2 C3 C2 C1 -0.3(2) . . . . ?
N10 N9 C15 C16 -0.6(3) . . . . ?
N10 C17 C16 C15 0.0(3) . . . . ?
N8 N7 C12 C13 -1.0(3) . . . . ?
N8 N7 C12 C21 179.0(2) . . . . ?
N8 C14 C13 C12 -0.7(3) . . . . ?
N1 N2 C3 C2 0.9(2) . . . . ?
N1 N2 C3 C11 -177.72(19) . . . . ?
N1 N2 B1 N6 61.1(2) . . . . ?
N1 N2 B1 N4 -55.3(2) . . . . ?
N1 C1 C2 C3 -0.4(2) . . . . ?
N11 N12 C20 C19 0.7(3) . . . . ?
N11 N12 B2 N10 59.6(2) . . . . ?
N11 N12 B2 N8 -57.1(2) . . . . ?
N11 C18 C19 C20 -0.3(3) . . . . ?
N6 N5 C7 C8 -0.8(3) . . . . ?
N6 C9 C8 C7 0.0(3) . . . . ?
N5 N6 C9 C8 -0.6(3) . . . . ?
N5 N6 B1 N2 -59.0(2) . . . . ?
N5 N6 B1 N4 58.1(2) . . . . ?
N5 C7 C8 C9 0.5(3) . . . . ?
N4 N3 C4 C5 -0.6(3) . . . . ?
N4 C6 C5 C4 0.4(3) . . . . ?
N12 N11 C18 C19 0.7(3) . . . . ?
N12 C20 C19 C18 -0.3(3) . . . . ?
N9 N10 C17 C16 -0.4(3) . . . . ?
N9 N10 B2 N8 56.0(2) . . . . ?
N9 N10 B2 N12 -60.6(2) . . . . ?
N9 C15 C16 C17 0.4(3) . . . . ?
N3 N4 C6 C5 -0.8(3) . . . . ?
N3 N4 B1 N2 55.5(2) . . . . ?
N3 N4 B1 N6 -60.3(2) . . . . ?
N3 C4 C5 C6 0.2(3) . . . . ?
C14 N8 B2 N10 120.6(2) . . . . ?
C14 N8 B2 N12 -123.1(2) . . . . ?
C14 C13 C12 N7 1.0(3) . . . . ?
C14 C13 C12 C21 -178.9(3) . . . . ?
C12 N7 N8 C14 0.5(2) . . . . ?
C12 N7 N8 B2 179.39(18) . . . . ?
C6 N4 N3 Fe01 -176.29(15) . . . . ?
C6 N4 N3 C4 0.8(2) . . . . ?
C6 N4 B1 N2 -123.8(2) . . . . ?
C6 N4 B1 N6 120.4(2) . . . . ?
C17 N10 N9 Fe02 -176.92(15) . . . . ?
C17 N10 N9 C15 0.6(2) . . . . ?
C17 N10 B2 N8 -122.5(2) . . . . ?
C17 N10 B2 N12 120.9(2) . . . . ?
C3 N2 N1 Fe01 174.43(13) . . . . ?
C3 N2 N1 C1 -1.1(2) . . . . ?
C3 N2 B1 N6 -115.7(2) . . . . ?
C3 N2 B1 N4 127.9(2) . . . . ?
C18 N11 N12 C20 -0.9(2) . . . . ?
C18 N11 N12 B2 -179.15(18) . . . . ?
C20 N12 B2 N10 -118.2(2) . . . . ?
C20 N12 B2 N8 125.1(2) . . . . ?
C9 N6 N5 Fe01 -175.86(14) . . . . ?
C9 N6 N5 C7 0.9(2) . . . . ?
C9 N6 B1 N2 114.0(2) . . . . ?
C9 N6 B1 N4 -128.8(2) . . . . ?
C22 C14 C13 C12 179.6(2) . . . . ?
C10 C1 C2 C3 179.7(2) . . . . ?
C11 C3 C2 C1 178.2(2) . . . . ?
B1 N2 N1 Fe01 -3.0(2) . . . . ?
B1 N2 N1 C1 -178.53(17) . . . . ?
B1 N2 C3 C2 177.9(2) . . . . ?
B1 N2 C3 C11 -0.7(3) . . . . ?
B1 N6 N5 Fe01 -1.3(2) . . . . ?
B1 N6 N5 C7 175.41(18) . . . . ?
B1 N6 C9 C8 -174.1(2) . . . . ?
B1 N4 N3 Fe01 4.2(2) . . . . ?
B1 N4 N3 C4 -178.63(19) . . . . ?
B1 N4 C6 C5 178.6(2) . . . . ?
B2 N10 N9 Fe02 4.3(2) . . . . ?
B2 N10 N9 C15 -178.21(19) . . . . ?
B2 N10 C17 C16 178.2(2) . . . . ?
B2 N8 C14 C13 -178.5(2) . . . . ?
B2 N8 C14 C22 1.2(4) . . . . ?
B2 N12 C20 C19 178.7(2) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_300K
_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_pr210_320k
_database_code_depnum_ccdc_archive 'CCDC 2261113'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9075(6)
_cell_length_b                   10.7822(6)
_cell_length_c                   12.2486(6)
_cell_angle_alpha                93.059(4)
_cell_angle_beta                 94.959(3)
_cell_angle_gamma                95.424(3)
_cell_volume                     1295.22(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5793
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.790
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11033
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         3.112
_diffrn_ambient_temperature      320(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 6 sets of ω scans each set at different φ and/or 2θ angles and each scan (120.00 s exposure) covering 2.000\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4346
_reflns_number_total             5885
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5885
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0405
_refine_ls_restrained_S_all      1.031
_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)+(0.0680P)²+0.1146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1198
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.04791(13) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.04914(13) Uani 1 2 d S . P . .
N7 N 0.80683(18) 1.00798(17) 0.92533(15) 0.0602(4) Uani 1 1 d . . . . .
N2 N 0.78168(17) 0.55342(16) 0.43733(13) 0.0552(4) Uani 1 1 d . . . . .
N10 N 0.86291(18) 0.74583(16) 0.96498(15) 0.0589(4) Uani 1 1 d . . . . .
N8 N 0.70797(17) 0.91376(17) 0.94189(15) 0.0585(4) Uani 1 1 d . . . . .
N1 N 0.69553(17) 0.58828(16) 0.51392(14) 0.0560(4) Uani 1 1 d . . . . .
N11 N 0.91025(19) 0.95629(17) 1.13734(15) 0.0601(4) Uani 1 1 d . . . . .
N6 N 0.60603(19) 0.48986(17) 0.28236(14) 0.0595(4) Uani 1 1 d . . . . .
N5 N 0.49666(18) 0.51821(17) 0.33539(14) 0.0590(4) Uani 1 1 d . . . . .
N4 N 0.68179(18) 0.33042(16) 0.40898(15) 0.0594(4) Uani 1 1 d . . . . .
N12 N 0.80169(18) 0.86700(16) 1.12912(15) 0.0587(4) Uani 1 1 d . . . . .
N9 N 0.97968(18) 0.81698(16) 0.94887(15) 0.0599(4) Uani 1 1 d . . . . .
N3 N 0.58511(19) 0.33761(16) 0.48126(15) 0.0601(4) Uani 1 1 d . . . . .
C14 C 0.5885(2) 0.9328(2) 0.88535(19) 0.0674(6) Uani 1 1 d . . . . .
C13 C 0.6115(3) 1.0399(3) 0.8321(2) 0.0793(7) Uani 1 1 d . . . . .
H13 H 0.548276 1.075812 0.786381 0.095 Uiso 1 1 calc R U . . .
C12 C 0.7470(2) 1.0851(2) 0.8590(2) 0.0705(6) Uani 1 1 d . . . . .
C4 C 0.5652(3) 0.2251(2) 0.5195(2) 0.0743(6) Uani 1 1 d . . . . .
H4 H 0.504600 0.203732 0.570969 0.089 Uiso 1 1 calc R U . . .
C6 C 0.7187(3) 0.2134(2) 0.4026(2) 0.0752(6) Uani 1 1 d . . . . .
H6 H 0.782151 0.184548 0.358206 0.090 Uiso 1 1 calc R U . . .
C17 C 0.8730(3) 0.6272(2) 0.9305(2) 0.0734(6) Uani 1 1 d . . . . .
H17 H 0.806438 0.560874 0.933516 0.088 Uiso 1 1 calc R U . . .
C5 C 0.6467(3) 0.1442(2) 0.4726(3) 0.0872(8) Uani 1 1 d . . . . .
H5 H 0.651732 0.060496 0.485716 0.105 Uiso 1 1 calc R U . . .
C3 C 0.9004(2) 0.6273(2) 0.45148(18) 0.0601(5) Uani 1 1 d . . . . .
C15 C 1.0592(3) 0.7400(2) 0.9032(2) 0.0744(6) Uani 1 1 d . . . . .
H15 H 1.145566 0.764141 0.882668 0.089 Uiso 1 1 calc R U . . .
C1 C 0.7643(2) 0.6835(2) 0.57621(18) 0.0620(5) Uani 1 1 d . . . . .
C2 C 0.8922(2) 0.7095(2) 0.5386(2) 0.0681(6) Uani 1 1 d . . . . .
H2 H 0.959405 0.771481 0.567540 0.082 Uiso 1 1 calc R U . . .
C16 C 0.9962(3) 0.6192(3) 0.8904(2) 0.0840(7) Uani 1 1 d . . . . .
H16 H 1.030265 0.548494 0.861044 0.101 Uiso 1 1 calc R U . . .
C18 C 0.9372(3) 0.9889(2) 1.2436(2) 0.0729(6) Uani 1 1 d . . . . .
H18 H 1.005987 1.049216 1.273010 0.087 Uiso 1 1 calc R U . . .
C7 C 0.4108(3) 0.5605(2) 0.2608(2) 0.0732(6) Uani 1 1 d . . . . .
H7 H 0.326355 0.585877 0.274427 0.088 Uiso 1 1 calc R U . . .
C20 C 0.7647(3) 0.8446(2) 1.2299(2) 0.0708(6) Uani 1 1 d . . . . .
H20 H 0.694083 0.787369 1.246022 0.085 Uiso 1 1 calc R U . . .
C9 C 0.5868(3) 0.5166(3) 0.17674(19) 0.0765(7) Uani 1 1 d . . . . .
H9 H 0.647540 0.506087 0.123982 0.092 Uiso 1 1 calc R U . . .
C19 C 0.8492(3) 0.9211(3) 1.3043(2) 0.0834(8) Uani 1 1 d . . . . .
H19 H 0.847623 0.926156 1.380203 0.100 Uiso 1 1 calc R U . . .
C21 C 0.8202(3) 1.2003(3) 0.8231(3) 0.0976(10) Uani 1 1 d . . . . .
H21A H 0.785010 1.272102 0.855622 0.146 Uiso 1 1 calc R U . . .
H21B H 0.807233 1.201093 0.744563 0.146 Uiso 1 1 calc R U . . .
H21C H 0.915544 1.202126 0.845875 0.146 Uiso 1 1 calc R U . . .
C8 C 0.4631(3) 0.5619(3) 0.1598(2) 0.0845(8) Uani 1 1 d . . . . .
H8 H 0.422924 0.587926 0.094610 0.101 Uiso 1 1 calc R U . . .
C22 C 0.4614(3) 0.8467(3) 0.8863(3) 0.0935(9) Uani 1 1 d . . . . .
H22A H 0.474508 0.766602 0.853102 0.140 Uiso 1 1 calc R U . . .
H22B H 0.387583 0.880543 0.845725 0.140 Uiso 1 1 calc R U . . .
H22C H 0.440367 0.837722 0.960699 0.140 Uiso 1 1 calc R U . . .
C10 C 0.7082(3) 0.7478(3) 0.6702(2) 0.0806(7) Uani 1 1 d . . . . .
H10A H 0.691635 0.830936 0.652241 0.121 Uiso 1 1 calc R U . . .
H10B H 0.772433 0.751540 0.733943 0.121 Uiso 1 1 calc R U . . .
H10C H 0.624361 0.702437 0.685135 0.121 Uiso 1 1 calc R U . . .
C11 C 1.0131(3) 0.6149(3) 0.3783(2) 0.0766(7) Uani 1 1 d . . . . .
H11A H 1.035957 0.530287 0.375680 0.115 Uiso 1 1 calc R U . . .
H11B H 1.091621 0.669776 0.406877 0.115 Uiso 1 1 calc R U . . .
H11C H 0.983723 0.636632 0.305705 0.115 Uiso 1 1 calc R U . . .
B1 B 0.7303(3) 0.4471(2) 0.3508(2) 0.0595(6) Uani 1 1 d . . . . .
B2 B 0.7465(3) 0.8086(2) 1.0147(2) 0.0588(6) Uani 1 1 d . . . . .
H1 H 0.810(2) 0.430(2) 0.2931(18) 0.063(6) Uiso 1 1 d . . . . .
H2A H 0.659(2) 0.738(2) 1.019(2) 0.071(7) Uiso 1 1 d . . . . .


_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 2.0652(17) . ?
Fe01 N1 2.0651(17) 2_666 ?
Fe01 N5 2.0339(17) 2_666 ?
Fe01 N5 2.0339(17) . ?
Fe01 N3 2.0246(18) . ?
Fe01 N3 2.0246(18) 2_666 ?
Fe02 N7 2.0599(18) . ?
Fe02 N7 2.0599(18) 2_777 ?
Fe02 N11 2.0264(18) . ?
Fe02 N11 2.0264(18) 2_777 ?
Fe02 N9 2.0244(18) 2_777 ?
Fe02 N9 2.0244(18) . ?
N7 N8 1.379(2) . ?
N7 C12 1.336(3) . ?
N2 N1 1.383(2) . ?
N2 C3 1.350(3) . ?
N2 B1 1.537(3) . ?
N10 N9 1.362(2) . ?
N10 C17 1.341(3) . ?
N10 B2 1.544(3) . ?
N8 C14 1.357(3) . ?
N8 B2 1.536(3) . ?
N1 C1 1.339(3) . ?
N11 N12 1.367(2) . ?
N11 C18 1.328(3) . ?
N6 N5 1.361(3) . ?
N6 C9 1.342(3) . ?
N6 B1 1.549(3) . ?
N5 C7 1.323(3) . ?
N4 N3 1.364(2) . ?
N4 C6 1.347(3) . ?
N4 B1 1.537(3) . ?
N12 C20 1.345(3) . ?
N12 B2 1.539(3) . ?
N9 C15 1.331(3) . ?
N3 C4 1.327(3) . ?
C14 C13 1.366(4) . ?
C14 C22 1.493(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.389(4) . ?
C12 C21 1.485(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.369(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.363(4) . ?
C5 H5 0.9300 . ?
C3 C2 1.363(3) . ?
C3 C11 1.501(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(4) . ?
C1 C2 1.395(3) . ?
C1 C10 1.488(3) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.378(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.382(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.367(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.365(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.13(2) . ?
B2 H2A 1.11(2) . ?

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 180.0 2_666 . ?
N5 Fe01 N1 92.52(7) . 2_666 ?
N5 Fe01 N1 87.48(7) 2_666 2_666 ?
N5 Fe01 N1 87.48(7) . . ?
N5 Fe01 N1 92.52(7) 2_666 . ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 93.10(7) 2_666 . ?
N3 Fe01 N1 93.10(7) . 2_666 ?
N3 Fe01 N1 86.90(7) 2_666 2_666 ?
N3 Fe01 N1 86.90(7) . . ?
N3 Fe01 N5 90.42(7) 2_666 . ?
N3 Fe01 N5 89.58(7) 2_666 2_666 ?
N3 Fe01 N5 90.42(7) . 2_666 ?
N3 Fe01 N5 89.58(7) . . ?
N3 Fe01 N3 180.00(9) . 2_666 ?
N7 Fe02 N7 180.0 2_777 . ?
N11 Fe02 N7 93.05(7) 2_777 . ?
N11 Fe02 N7 86.95(7) . . ?
N11 Fe02 N7 93.05(7) . 2_777 ?
N11 Fe02 N7 86.95(7) 2_777 2_777 ?
N11 Fe02 N11 180.0 2_777 . ?
N9 Fe02 N7 93.02(7) . 2_777 ?
N9 Fe02 N7 86.98(7) . . ?
N9 Fe02 N7 86.98(7) 2_777 2_777 ?
N9 Fe02 N7 93.02(7) 2_777 . ?
N9 Fe02 N11 90.32(7) 2_777 . ?
N9 Fe02 N11 89.68(7) . . ?
N9 Fe02 N11 90.32(7) . 2_777 ?
N9 Fe02 N11 89.68(7) 2_777 2_777 ?
N9 Fe02 N9 180.00(10) . 2_777 ?
N8 N7 Fe02 117.96(12) . . ?
C12 N7 Fe02 135.65(16) . . ?
C12 N7 N8 106.39(18) . . ?
N1 N2 B1 118.78(16) . . ?
C3 N2 N1 110.24(17) . . ?
C3 N2 B1 130.92(18) . . ?
N9 N10 B2 119.17(17) . . ?
C17 N10 N9 109.26(19) . . ?
C17 N10 B2 131.56(19) . . ?
N7 N8 B2 118.81(17) . . ?
C14 N8 N7 109.94(18) . . ?
C14 N8 B2 131.24(19) . . ?
N2 N1 Fe01 117.62(12) . . ?
C1 N1 Fe01 136.06(15) . . ?
C1 N1 N2 106.08(17) . . ?
N12 N11 Fe02 119.03(13) . . ?
C18 N11 Fe02 134.62(18) . . ?
C18 N11 N12 106.16(19) . . ?
N5 N6 B1 118.36(16) . . ?
C9 N6 N5 109.5(2) . . ?
C9 N6 B1 131.8(2) . . ?
N6 N5 Fe01 119.27(13) . . ?
C7 N5 Fe01 134.48(17) . . ?
C7 N5 N6 106.13(19) . . ?
N3 N4 B1 119.59(17) . . ?
C6 N4 N3 109.37(19) . . ?
C6 N4 B1 131.0(2) . . ?
N11 N12 B2 118.75(16) . . ?
C20 N12 N11 109.6(2) . . ?
C20 N12 B2 131.6(2) . . ?
N10 N9 Fe02 118.82(13) . . ?
C15 N9 Fe02 135.02(17) . . ?
C15 N9 N10 106.10(19) . . ?
N4 N3 Fe01 118.35(13) . . ?
C4 N3 Fe01 135.14(17) . . ?
C4 N3 N4 106.39(19) . . ?
N8 C14 C13 106.9(2) . . ?
N8 C14 C22 123.0(2) . . ?
C13 C14 C22 130.1(2) . . ?
C14 C13 H13 126.4 . . ?
C14 C13 C12 107.2(2) . . ?
C12 C13 H13 126.4 . . ?
N7 C12 C13 109.5(2) . . ?
N7 C12 C21 122.8(2) . . ?
C13 C12 C21 127.7(2) . . ?
N3 C4 H4 124.6 . . ?
N3 C4 C5 110.7(2) . . ?
C5 C4 H4 124.6 . . ?
N4 C6 H6 125.9 . . ?
N4 C6 C5 108.2(2) . . ?
C5 C6 H6 125.9 . . ?
N10 C17 H17 125.4 . . ?
N10 C17 C16 109.2(2) . . ?
C16 C17 H17 125.4 . . ?
C4 C5 H5 127.4 . . ?
C6 C5 C4 105.3(2) . . ?
C6 C5 H5 127.4 . . ?
N2 C3 C2 107.1(2) . . ?
N2 C3 C11 122.7(2) . . ?
C2 C3 C11 130.1(2) . . ?
N9 C15 H15 124.5 . . ?
N9 C15 C16 110.9(2) . . ?
C16 C15 H15 124.5 . . ?
N1 C1 C2 109.3(2) . . ?
N1 C1 C10 123.4(2) . . ?
C2 C1 C10 127.3(2) . . ?
C3 C2 C1 107.3(2) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C17 C16 C15 104.5(2) . . ?
C17 C16 H16 127.8 . . ?
C15 C16 H16 127.8 . . ?
N11 C18 H18 124.7 . . ?
N11 C18 C19 110.5(2) . . ?
C19 C18 H18 124.7 . . ?
N5 C7 H7 124.5 . . ?
N5 C7 C8 111.0(2) . . ?
C8 C7 H7 124.5 . . ?
N12 C20 H20 126.1 . . ?
N12 C20 C19 107.9(2) . . ?
C19 C20 H20 126.1 . . ?
N6 C9 H9 125.7 . . ?
N6 C9 C8 108.5(2) . . ?
C8 C9 H9 125.7 . . ?
C18 C19 H19 127.1 . . ?
C20 C19 C18 105.8(2) . . ?
C20 C19 H19 127.1 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.6 . . ?
C9 C8 C7 104.8(2) . . ?
C9 C8 H8 127.6 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 107.14(18) . . ?
N2 B1 H1 111.3(11) . . ?
N6 B1 H1 107.7(11) . . ?
N4 B1 N2 109.22(18) . . ?
N4 B1 N6 108.21(18) . . ?
N4 B1 H1 113.0(11) . . ?
N10 B2 H2A 109.3(13) . . ?
N8 B2 N10 108.15(17) . . ?
N8 B2 N12 108.40(18) . . ?
N8 B2 H2A 111.5(13) . . ?
N12 B2 N10 107.70(18) . . ?
N12 B2 H2A 111.6(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -173.21(16) . . . . ?
Fe01 N1 C1 C10 6.9(4) . . . . ?
Fe01 N5 C7 C8 174.94(17) . . . . ?
Fe01 N3 C4 C5 175.26(19) . . . . ?
Fe02 N7 N8 C14 -178.90(14) . . . . ?
Fe02 N7 N8 B2 0.1(2) . . . . ?
Fe02 N7 C12 C13 178.33(18) . . . . ?
Fe02 N7 C12 C21 -1.8(4) . . . . ?
Fe02 N11 N12 C20 174.87(14) . . . . ?
Fe02 N11 N12 B2 -3.5(2) . . . . ?
Fe02 N11 C18 C19 -173.93(18) . . . . ?
Fe02 N9 C15 C16 176.43(18) . . . . ?
N7 N8 C14 C13 0.1(3) . . . . ?
N7 N8 C14 C22 179.9(2) . . . . ?
N7 N8 B2 N10 -58.2(2) . . . . ?
N7 N8 B2 N12 58.4(2) . . . . ?
N2 N1 C1 C2 0.7(2) . . . . ?
N2 N1 C1 C10 -179.2(2) . . . . ?
N2 C3 C2 C1 -0.4(2) . . . . ?
N10 N9 C15 C16 -0.6(3) . . . . ?
N10 C17 C16 C15 0.1(3) . . . . ?
N8 N7 C12 C13 -0.8(3) . . . . ?
N8 N7 C12 C21 179.0(2) . . . . ?
N8 C14 C13 C12 -0.6(3) . . . . ?
N1 N2 C3 C2 0.8(2) . . . . ?
N1 N2 C3 C11 -178.1(2) . . . . ?
N1 N2 B1 N6 61.6(2) . . . . ?
N1 N2 B1 N4 -55.4(2) . . . . ?
N1 C1 C2 C3 -0.2(3) . . . . ?
N11 N12 C20 C19 0.6(3) . . . . ?
N11 N12 B2 N10 60.0(2) . . . . ?
N11 N12 B2 N8 -56.8(2) . . . . ?
N11 C18 C19 C20 -0.5(3) . . . . ?
N6 N5 C7 C8 -0.8(3) . . . . ?
N6 C9 C8 C7 0.1(3) . . . . ?
N5 N6 C9 C8 -0.6(3) . . . . ?
N5 N6 B1 N2 -59.4(2) . . . . ?
N5 N6 B1 N4 58.3(2) . . . . ?
N5 C7 C8 C9 0.5(3) . . . . ?
N4 N3 C4 C5 -0.5(3) . . . . ?
N4 C6 C5 C4 0.5(3) . . . . ?
N12 N11 C18 C19 0.8(3) . . . . ?
N12 C20 C19 C18 -0.1(3) . . . . ?
N9 N10 C17 C16 -0.5(3) . . . . ?
N9 N10 B2 N8 56.5(2) . . . . ?
N9 N10 B2 N12 -60.4(2) . . . . ?
N9 C15 C16 C17 0.3(3) . . . . ?
N3 N4 C6 C5 -0.9(3) . . . . ?
N3 N4 B1 N2 55.7(2) . . . . ?
N3 N4 B1 N6 -60.6(2) . . . . ?
N3 C4 C5 C6 0.0(3) . . . . ?
C14 N8 B2 N10 120.6(2) . . . . ?
C14 N8 B2 N12 -122.9(2) . . . . ?
C14 C13 C12 N7 0.9(3) . . . . ?
C14 C13 C12 C21 -178.9(3) . . . . ?
C12 N7 N8 C14 0.4(2) . . . . ?
C12 N7 N8 B2 179.4(2) . . . . ?
C6 N4 N3 Fe01 -175.76(15) . . . . ?
C6 N4 N3 C4 0.8(3) . . . . ?
C6 N4 B1 N2 -124.2(2) . . . . ?
C6 N4 B1 N6 119.5(2) . . . . ?
C17 N10 N9 Fe02 -176.92(16) . . . . ?
C17 N10 N9 C15 0.7(2) . . . . ?
C17 N10 B2 N8 -122.4(2) . . . . ?
C17 N10 B2 N12 120.6(2) . . . . ?
C3 N2 N1 Fe01 174.29(13) . . . . ?
C3 N2 N1 C1 -0.9(2) . . . . ?
C3 N2 B1 N6 -115.3(2) . . . . ?
C3 N2 B1 N4 127.7(2) . . . . ?
C18 N11 N12 C20 -0.9(2) . . . . ?
C18 N11 N12 B2 -179.3(2) . . . . ?
C20 N12 B2 N10 -118.0(2) . . . . ?
C20 N12 B2 N8 125.2(2) . . . . ?
C9 N6 N5 Fe01 -175.68(15) . . . . ?
C9 N6 N5 C7 0.9(2) . . . . ?
C9 N6 B1 N2 113.6(3) . . . . ?
C9 N6 B1 N4 -128.7(2) . . . . ?
C22 C14 C13 C12 179.6(3) . . . . ?
C10 C1 C2 C3 179.6(2) . . . . ?
C11 C3 C2 C1 178.4(2) . . . . ?
B1 N2 N1 Fe01 -3.2(2) . . . . ?
B1 N2 N1 C1 -178.44(18) . . . . ?
B1 N2 C3 C2 177.9(2) . . . . ?
B1 N2 C3 C11 -1.0(3) . . . . ?
B1 N6 N5 Fe01 -1.2(2) . . . . ?
B1 N6 N5 C7 175.35(19) . . . . ?
B1 N6 C9 C8 -174.1(2) . . . . ?
B1 N4 N3 Fe01 4.4(2) . . . . ?
B1 N4 N3 C4 -179.0(2) . . . . ?
B1 N4 C6 C5 179.0(2) . . . . ?
B2 N10 N9 Fe02 3.9(2) . . . . ?
B2 N10 N9 C15 -178.5(2) . . . . ?
B2 N10 C17 C16 178.5(2) . . . . ?
B2 N8 C14 C13 -178.7(2) . . . . ?
B2 N8 C14 C22 1.1(4) . . . . ?
B2 N12 C20 C19 178.7(2) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_320K
_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_pr210_380k
_database_code_depnum_ccdc_archive 'CCDC 2261118'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0087(7)
_cell_length_b                   10.9499(8)
_cell_length_c                   12.3131(9)
_cell_angle_alpha                93.042(5)
_cell_angle_beta                 95.035(5)
_cell_angle_gamma                95.212(5)
_cell_volume                     1336.14(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5209
_cell_measurement_temperature    380(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.795
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10187
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         3.499
_diffrn_ambient_temperature      380(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 3 sets of ω scans each set at different φ and/or 2θ angles and each scan (240.00 s exposure) covering 2.000\ degrees in ω.
The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3967
_reflns_number_total             6028
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6028
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.019
_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)+(0.0773P)²+0.0493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1378
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.06242(16) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.06507(16) Uani 1 2 d S . P . .
N7 N 0.8007(2) 1.00513(19) 0.92250(18) 0.0795(5) Uani 1 1 d . . . . .
N2 N 0.78417(19) 0.55340(18) 0.43542(15) 0.0717(5) Uani 1 1 d . . . . .
N10 N 0.8603(2) 0.74540(17) 0.96484(17) 0.0749(5) Uani 1 1 d . . . . .
N8 N 0.70501(19) 0.91135(19) 0.94079(17) 0.0755(5) Uani 1 1 d . . . . .
N1 N 0.70088(19) 0.58900(18) 0.51250(16) 0.0729(5) Uani 1 1 d . . . . .
N11 N 0.9030(2) 0.95440(19) 1.14014(17) 0.0780(5) Uani 1 1 d . . . . .
N6 N 0.6101(2) 0.49016(19) 0.28025(16) 0.0751(5) Uani 1 1 d . . . . .
N5 N 0.4991(2) 0.51661(19) 0.32973(16) 0.0768(5) Uani 1 1 d . . . . .
N4 N 0.6865(2) 0.33293(18) 0.40725(17) 0.0756(5) Uani 1 1 d . . . . .
N12 N 0.7980(2) 0.86590(18) 1.12857(17) 0.0745(5) Uani 1 1 d . . . . .
N9 N 0.9772(2) 0.81219(18) 0.94882(18) 0.0790(5) Uani 1 1 d . . . . .
N3 N 0.5919(2) 0.33628(19) 0.48036(17) 0.0787(5) Uani 1 1 d . . . . .
C14 C 0.5860(3) 0.9279(3) 0.8854(2) 0.0852(7) Uani 1 1 d . . . . .
C13 C 0.6054(3) 1.0315(3) 0.8301(3) 0.1012(9) Uani 1 1 d . . . . .
H13 H 0.541308 1.064694 0.784045 0.121 Uiso 1 1 calc R U . . .
C12 C 0.7384(3) 1.0781(3) 0.8554(2) 0.0887(7) Uani 1 1 d . . . . .
C4 C 0.5754(3) 0.2235(3) 0.5161(3) 0.0970(8) Uani 1 1 d . . . . .
H4 H 0.516861 0.199951 0.567539 0.116 Uiso 1 1 calc R U . . .
C6 C 0.7242(3) 0.2179(3) 0.3984(3) 0.0964(8) Uani 1 1 d . . . . .
H6 H 0.786492 0.191406 0.352745 0.116 Uiso 1 1 calc R U . . .
C17 C 0.8674(3) 0.6285(2) 0.9320(2) 0.0949(8) Uani 1 1 d . . . . .
H17 H 0.799793 0.564984 0.935401 0.114 Uiso 1 1 calc R U . . .
C5 C 0.6566(4) 0.1469(3) 0.4667(3) 0.1105(10) Uani 1 1 d . . . . .
H5 H 0.663642 0.064282 0.477727 0.133 Uiso 1 1 calc R U . . .
C3 C 0.9022(2) 0.6251(2) 0.4477(2) 0.0760(6) Uani 1 1 d . . . . .
C15 C 1.0533(3) 0.7329(3) 0.9044(3) 0.0958(8) Uani 1 1 d . . . . .
H15 H 1.139241 0.753860 0.883809 0.115 Uiso 1 1 calc R U . . .
C1 C 0.7706(3) 0.6834(2) 0.5721(2) 0.0787(6) Uani 1 1 d . . . . .
C2 C 0.8958(3) 0.7074(3) 0.5335(2) 0.0860(7) Uani 1 1 d . . . . .
H2 H 0.962818 0.768387 0.561000 0.103 Uiso 1 1 calc R U . . .
C16 C 0.9885(4) 0.6163(3) 0.8930(3) 0.1077(10) Uani 1 1 d . . . . .
H16 H 1.020362 0.545094 0.864833 0.129 Uiso 1 1 calc R U . . .
C18 C 0.9259(3) 0.9835(3) 1.2467(2) 0.0942(8) Uani 1 1 d . . . . .
H18 H 0.992306 1.042863 1.278256 0.113 Uiso 1 1 calc R U . . .
C7 C 0.4163(3) 0.5578(3) 0.2525(2) 0.0914(8) Uani 1 1 d . . . . .
H7 H 0.331888 0.582882 0.263351 0.110 Uiso 1 1 calc R U . . .
C20 C 0.7589(3) 0.8407(3) 1.2272(2) 0.0874(7) Uani 1 1 d . . . . .
H20 H 0.689189 0.782932 1.240624 0.105 Uiso 1 1 calc R U . . .
C9 C 0.5944(3) 0.5153(3) 0.1756(2) 0.0929(8) Uani 1 1 d . . . . .
H9 H 0.657050 0.505036 0.125171 0.111 Uiso 1 1 calc R U . . .
C19 C 0.8384(4) 0.9140(3) 1.3038(3) 0.1043(10) Uani 1 1 d . . . . .
H19 H 0.834541 0.916601 1.379103 0.125 Uiso 1 1 calc R U . . .
C21 C 0.8098(4) 1.1914(3) 0.8181(3) 0.1254(13) Uani 1 1 d . . . . .
H21A H 0.800038 1.259794 0.867899 0.188 Uiso 1 1 calc R U . . .
H21B H 0.771668 1.206807 0.746432 0.188 Uiso 1 1 calc R U . . .
H21C H 0.903622 1.180517 0.816005 0.188 Uiso 1 1 calc R U . . .
C8 C 0.4726(4) 0.5583(3) 0.1543(2) 0.1037(10) Uani 1 1 d . . . . .
H8 H 0.435231 0.582760 0.088036 0.124 Uiso 1 1 calc R U . . .
C22 C 0.4608(3) 0.8422(4) 0.8883(3) 0.1221(12) Uani 1 1 d . . . . .
H22A H 0.470678 0.766002 0.848862 0.183 Uiso 1 1 calc R U . . .
H22B H 0.384904 0.878628 0.855065 0.183 Uiso 1 1 calc R U . . .
H22C H 0.446777 0.827070 0.962701 0.183 Uiso 1 1 calc R U . . .
C10 C 0.7146(3) 0.7484(3) 0.6653(2) 0.1025(9) Uani 1 1 d . . . . .
H10A H 0.689323 0.826719 0.643824 0.154 Uiso 1 1 calc R U . . .
H10B H 0.781697 0.760318 0.726599 0.154 Uiso 1 1 calc R U . . .
H10C H 0.636859 0.699872 0.685429 0.154 Uiso 1 1 calc R U . . .
C11 C 1.0132(3) 0.6118(3) 0.3748(3) 0.0982(8) Uani 1 1 d . . . . .
H11A H 1.036448 0.528660 0.373206 0.147 Uiso 1 1 calc R U . . .
H11B H 1.090676 0.666423 0.402192 0.147 Uiso 1 1 calc R U . . .
H11C H 0.983353 0.631904 0.302188 0.147 Uiso 1 1 calc R U . . .
B1 B 0.7329(3) 0.4479(3) 0.3503(2) 0.0756(7) Uani 1 1 d . . . . .
B2 B 0.7450(3) 0.8089(3) 1.0141(2) 0.0754(7) Uani 1 1 d . . . . .
H1 H 0.805(2) 0.429(2) 0.2922(19) 0.078(7) Uiso 1 1 d . . . . .
H2A H 0.658(3) 0.740(2) 1.017(2) 0.081(7) Uiso 1 1 d . . . . .


_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 2.1423(19) 2_666 ?
Fe01 N1 2.1423(19) . ?
Fe01 N5 2.113(2) 2_666 ?
Fe01 N5 2.113(2) . ?
Fe01 N3 2.100(2) . ?
Fe01 N3 2.100(2) 2_666 ?
Fe02 N7 2.142(2) 2_777 ?
Fe02 N7 2.141(2) . ?
Fe02 N11 2.113(2) . ?
Fe02 N11 2.113(2) 2_777 ?
Fe02 N9 2.105(2) 2_777 ?
Fe02 N9 2.105(2) . ?
N7 N8 1.380(3) . ?
N7 C12 1.335(3) . ?
N2 N1 1.381(3) . ?
N2 C3 1.350(3) . ?
N2 B1 1.538(3) . ?
N10 N9 1.357(3) . ?
N10 C17 1.332(3) . ?
N10 B2 1.552(4) . ?
N8 C14 1.351(3) . ?
N8 B2 1.536(4) . ?
N1 C1 1.339(3) . ?
N11 N12 1.356(3) . ?
N11 C18 1.328(4) . ?
N6 N5 1.359(3) . ?
N6 C9 1.331(3) . ?
N6 B1 1.558(4) . ?
N5 C7 1.330(3) . ?
N4 N3 1.364(3) . ?
N4 C6 1.350(3) . ?
N4 B1 1.528(4) . ?
N12 C20 1.343(3) . ?
N12 B2 1.540(4) . ?
N9 C15 1.333(3) . ?
N3 C4 1.334(3) . ?
C14 C13 1.361(4) . ?
C14 C22 1.500(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.384(4) . ?
C12 C21 1.488(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.375(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.358(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.358(4) . ?
C5 H5 0.9300 . ?
C3 C2 1.361(4) . ?
C3 C11 1.501(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.373(4) . ?
C1 C2 1.387(4) . ?
C1 C10 1.495(4) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.373(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.378(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.357(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.356(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.09(2) . ?
B2 H2A 1.10(2) . ?

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 180.0 . 2_666 ?
N5 Fe01 N1 86.45(8) . . ?
N5 Fe01 N1 93.55(8) 2_666 . ?
N5 Fe01 N1 93.55(8) . 2_666 ?
N5 Fe01 N1 86.45(8) 2_666 2_666 ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 85.30(8) 2_666 2_666 ?
N3 Fe01 N1 85.31(8) . . ?
N3 Fe01 N1 94.70(8) 2_666 . ?
N3 Fe01 N1 94.70(8) . 2_666 ?
N3 Fe01 N5 91.64(8) 2_666 . ?
N3 Fe01 N5 88.35(8) 2_666 2_666 ?
N3 Fe01 N5 91.65(8) . 2_666 ?
N3 Fe01 N5 88.36(8) . . ?
N3 Fe01 N3 180.0 . 2_666 ?
N7 Fe02 N7 180.0 . 2_777 ?
N11 Fe02 N7 85.35(8) 2_777 2_777 ?
N11 Fe02 N7 94.65(8) . 2_777 ?
N11 Fe02 N7 85.35(8) . . ?
N11 Fe02 N7 94.65(8) 2_777 . ?
N11 Fe02 N11 180.0 2_777 . ?
N9 Fe02 N7 85.70(8) . . ?
N9 Fe02 N7 94.30(8) . 2_777 ?
N9 Fe02 N7 94.30(8) 2_777 . ?
N9 Fe02 N7 85.70(8) 2_777 2_777 ?
N9 Fe02 N11 91.57(8) 2_777 . ?
N9 Fe02 N11 88.43(8) . . ?
N9 Fe02 N11 91.57(8) . 2_777 ?
N9 Fe02 N11 88.43(8) 2_777 2_777 ?
N9 Fe02 N9 180.0 . 2_777 ?
N8 N7 Fe02 117.45(14) . . ?
C12 N7 Fe02 136.45(18) . . ?
C12 N7 N8 106.1(2) . . ?
N1 N2 B1 119.32(18) . . ?
C3 N2 N1 110.3(2) . . ?
C3 N2 B1 130.4(2) . . ?
N9 N10 B2 120.12(18) . . ?
C17 N10 N9 109.3(2) . . ?
C17 N10 B2 130.6(2) . . ?
N7 N8 B2 119.45(19) . . ?
C14 N8 N7 109.8(2) . . ?
C14 N8 B2 130.7(2) . . ?
N2 N1 Fe01 117.28(14) . . ?
C1 N1 Fe01 136.69(17) . . ?
C1 N1 N2 105.69(19) . . ?
N12 N11 Fe02 118.27(15) . . ?
C18 N11 Fe02 135.5(2) . . ?
C18 N11 N12 105.9(2) . . ?
N5 N6 B1 119.17(18) . . ?
C9 N6 N5 109.6(2) . . ?
C9 N6 B1 131.1(2) . . ?
N6 N5 Fe01 118.55(15) . . ?
C7 N5 Fe01 135.46(19) . . ?
C7 N5 N6 105.8(2) . . ?
N3 N4 B1 120.91(19) . . ?
C6 N4 N3 108.7(2) . . ?
C6 N4 B1 130.4(2) . . ?
N11 N12 B2 119.95(19) . . ?
C20 N12 N11 109.7(2) . . ?
C20 N12 B2 130.4(2) . . ?
N10 N9 Fe02 118.19(15) . . ?
C15 N9 Fe02 136.14(19) . . ?
C15 N9 N10 105.6(2) . . ?
N4 N3 Fe01 117.39(15) . . ?
C4 N3 Fe01 136.1(2) . . ?
C4 N3 N4 106.3(2) . . ?
N8 C14 C13 107.3(2) . . ?
N8 C14 C22 123.2(3) . . ?
C13 C14 C22 129.4(3) . . ?
C14 C13 H13 126.5 . . ?
C14 C13 C12 107.1(2) . . ?
C12 C13 H13 126.5 . . ?
N7 C12 C13 109.7(3) . . ?
N7 C12 C21 121.7(3) . . ?
C13 C12 C21 128.6(3) . . ?
N3 C4 H4 124.6 . . ?
N3 C4 C5 110.8(3) . . ?
C5 C4 H4 124.6 . . ?
N4 C6 H6 125.5 . . ?
N4 C6 C5 109.0(3) . . ?
C5 C6 H6 125.5 . . ?
N10 C17 H17 125.3 . . ?
N10 C17 C16 109.5(3) . . ?
C16 C17 H17 125.3 . . ?
C4 C5 H5 127.4 . . ?
C6 C5 C4 105.2(3) . . ?
C6 C5 H5 127.4 . . ?
N2 C3 C2 107.1(2) . . ?
N2 C3 C11 123.4(2) . . ?
C2 C3 C11 129.5(2) . . ?
N9 C15 H15 124.4 . . ?
N9 C15 C16 111.2(3) . . ?
C16 C15 H15 124.4 . . ?
N1 C1 C2 109.7(2) . . ?
N1 C1 C10 122.3(2) . . ?
C2 C1 C10 128.0(2) . . ?
C3 C2 C1 107.1(2) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C17 C16 C15 104.3(3) . . ?
C17 C16 H16 127.8 . . ?
C15 C16 H16 127.8 . . ?
N11 C18 H18 124.6 . . ?
N11 C18 C19 110.9(3) . . ?
C19 C18 H18 124.6 . . ?
N5 C7 H7 124.6 . . ?
N5 C7 C8 110.8(3) . . ?
C8 C7 H7 124.6 . . ?
N12 C20 H20 125.9 . . ?
N12 C20 C19 108.3(3) . . ?
C19 C20 H20 125.9 . . ?
N6 C9 H9 125.5 . . ?
N6 C9 C8 109.1(3) . . ?
C8 C9 H9 125.5 . . ?
C18 C19 H19 127.3 . . ?
C20 C19 C18 105.3(3) . . ?
C20 C19 H19 127.3 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.6 . . ?
C9 C8 C7 104.8(3) . . ?
C9 C8 H8 127.6 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 107.3(2) . . ?
N2 B1 H1 113.4(12) . . ?
N6 B1 H1 105.1(12) . . ?
N4 B1 N2 110.2(2) . . ?
N4 B1 N6 108.9(2) . . ?
N4 B1 H1 111.5(12) . . ?
N10 B2 H2A 108.9(13) . . ?
N8 B2 N10 108.7(2) . . ?
N8 B2 N12 109.2(2) . . ?
N8 B2 H2A 109.9(13) . . ?
N12 B2 N10 108.3(2) . . ?
N12 B2 H2A 111.7(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -172.72(19) . . . . ?
Fe01 N1 C1 C10 7.3(4) . . . . ?
Fe01 N5 C7 C8 174.0(2) . . . . ?
Fe01 N3 C4 C5 173.3(2) . . . . ?
Fe02 N7 N8 C14 -179.43(17) . . . . ?
Fe02 N7 N8 B2 -0.3(3) . . . . ?
Fe02 N7 C12 C13 178.5(2) . . . . ?
Fe02 N7 C12 C21 -1.8(5) . . . . ?
Fe02 N11 N12 C20 173.57(16) . . . . ?
Fe02 N11 N12 B2 -4.9(3) . . . . ?
Fe02 N11 C18 C19 -172.1(2) . . . . ?
Fe02 N9 C15 C16 176.6(2) . . . . ?
N7 N8 C14 C13 0.9(3) . . . . ?
N7 N8 C14 C22 -179.7(3) . . . . ?
N7 N8 B2 N10 -58.7(3) . . . . ?
N7 N8 B2 N12 59.3(3) . . . . ?
N2 N1 C1 C2 0.1(3) . . . . ?
N2 N1 C1 C10 -179.9(2) . . . . ?
N2 C3 C2 C1 -0.2(3) . . . . ?
N10 N9 C15 C16 -0.8(3) . . . . ?
N10 C17 C16 C15 0.0(4) . . . . ?
N8 N7 C12 C13 -0.6(3) . . . . ?
N8 N7 C12 C21 179.2(3) . . . . ?
N8 C14 C13 C12 -1.2(3) . . . . ?
N1 N2 C3 C2 0.2(3) . . . . ?
N1 N2 C3 C11 -178.5(2) . . . . ?
N1 N2 B1 N6 63.0(3) . . . . ?
N1 N2 B1 N4 -55.5(3) . . . . ?
N1 C1 C2 C3 0.0(3) . . . . ?
N11 N12 C20 C19 0.4(3) . . . . ?
N11 N12 B2 N10 61.5(3) . . . . ?
N11 N12 B2 N8 -56.8(3) . . . . ?
N11 C18 C19 C20 -0.5(4) . . . . ?
N6 N5 C7 C8 -0.1(3) . . . . ?
N6 C9 C8 C7 0.2(3) . . . . ?
N5 N6 C9 C8 -0.2(3) . . . . ?
N5 N6 B1 N2 -61.5(3) . . . . ?
N5 N6 B1 N4 57.8(3) . . . . ?
N5 C7 C8 C9 -0.1(4) . . . . ?
N4 N3 C4 C5 -0.6(3) . . . . ?
N4 C6 C5 C4 0.7(4) . . . . ?
N12 N11 C18 C19 0.8(3) . . . . ?
N12 C20 C19 C18 0.0(3) . . . . ?
N9 N10 C17 C16 -0.5(3) . . . . ?
N9 N10 B2 N8 58.0(3) . . . . ?
N9 N10 B2 N12 -60.6(3) . . . . ?
N9 C15 C16 C17 0.5(4) . . . . ?
N3 N4 C6 C5 -1.1(3) . . . . ?
N3 N4 B1 N2 55.4(3) . . . . ?
N3 N4 B1 N6 -62.1(3) . . . . ?
N3 C4 C5 C6 -0.1(4) . . . . ?
C14 N8 B2 N10 120.2(3) . . . . ?
C14 N8 B2 N12 -121.8(3) . . . . ?
C14 C13 C12 N7 1.1(4) . . . . ?
C14 C13 C12 C21 -178.6(3) . . . . ?
C12 N7 N8 C14 -0.2(3) . . . . ?
C12 N7 N8 B2 178.9(2) . . . . ?
C6 N4 N3 Fe01 -174.21(18) . . . . ?
C6 N4 N3 C4 1.0(3) . . . . ?
C6 N4 B1 N2 -124.7(3) . . . . ?
C6 N4 B1 N6 117.7(3) . . . . ?
C17 N10 N9 Fe02 -177.15(18) . . . . ?
C17 N10 N9 C15 0.8(3) . . . . ?
C17 N10 B2 N8 -121.7(3) . . . . ?
C17 N10 B2 N12 119.8(3) . . . . ?
C3 N2 N1 Fe01 174.26(15) . . . . ?
C3 N2 N1 C1 -0.2(3) . . . . ?
C3 N2 B1 N6 -114.6(3) . . . . ?
C3 N2 B1 N4 126.9(2) . . . . ?
C18 N11 N12 C20 -0.7(3) . . . . ?
C18 N11 N12 B2 -179.2(2) . . . . ?
C20 N12 B2 N10 -116.6(3) . . . . ?
C20 N12 B2 N8 125.1(3) . . . . ?
C9 N6 N5 Fe01 -175.09(17) . . . . ?
C9 N6 N5 C7 0.2(3) . . . . ?
C9 N6 B1 N2 112.8(3) . . . . ?
C9 N6 B1 N4 -127.8(3) . . . . ?
C22 C14 C13 C12 179.5(3) . . . . ?
C10 C1 C2 C3 -180.0(3) . . . . ?
C11 C3 C2 C1 178.5(3) . . . . ?
B1 N2 N1 Fe01 -3.8(3) . . . . ?
B1 N2 N1 C1 -178.3(2) . . . . ?
B1 N2 C3 C2 178.0(3) . . . . ?
B1 N2 C3 C11 -0.7(4) . . . . ?
B1 N6 N5 Fe01 0.4(3) . . . . ?
B1 N6 N5 C7 175.7(2) . . . . ?
B1 N6 C9 C8 -175.0(3) . . . . ?
B1 N4 N3 Fe01 5.7(3) . . . . ?
B1 N4 N3 C4 -179.1(2) . . . . ?
B1 N4 C6 C5 179.0(3) . . . . ?
B2 N10 N9 Fe02 3.1(3) . . . . ?
B2 N10 N9 C15 -178.9(2) . . . . ?
B2 N10 C17 C16 179.2(3) . . . . ?
B2 N8 C14 C13 -178.1(3) . . . . ?
B2 N8 C14 C22 1.2(5) . . . . ?
B2 N12 C20 C19 178.7(3) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_380K
_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_pr210_340k
_database_code_depnum_ccdc_archive 'CCDC 2261115'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9492(5)
_cell_length_b                   10.8446(5)
_cell_length_c                   12.2727(5)
_cell_angle_alpha                93.048(3)
_cell_angle_beta                 94.995(3)
_cell_angle_gamma                95.353(3)
_cell_volume                     1310.87(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5107
_cell_measurement_temperature    340(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11120
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         3.179
_diffrn_ambient_temperature      340(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.076209
_diffrn_orient_matrix_UB_12      0.065289
_diffrn_orient_matrix_UB_13      0.023627
_diffrn_orient_matrix_UB_21      0.006923
_diffrn_orient_matrix_UB_22      0.019672
_diffrn_orient_matrix_UB_23      -0.078122
_diffrn_orient_matrix_UB_31      -0.066509
_diffrn_orient_matrix_UB_32      0.062936
_diffrn_orient_matrix_UB_33      0.007376
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 6 sets of ω scans each set at different φ and/or 2θ angles and each scan (240.00 s exposure) covering 2.000\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4381
_reflns_number_total             5952
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.035
_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)+(0.0702P)²+0.1629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1248
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.05307(13) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.05488(13) Uani 1 2 d S . P . .
N7 N 0.80405(18) 1.00706(17) 0.92431(16) 0.0682(4) Uani 1 1 d . . . . .
N2 N 0.78289(17) 0.55325(16) 0.43668(14) 0.0621(4) Uani 1 1 d . . . . .
N10 N 0.86167(18) 0.74577(16) 0.96493(15) 0.0649(4) Uani 1 1 d . . . . .
N8 N 0.70667(17) 0.91269(17) 0.94155(15) 0.0651(4) Uani 1 1 d . . . . .
N1 N 0.69765(17) 0.58858(16) 0.51341(14) 0.0625(4) Uani 1 1 d . . . . .
N11 N 0.90744(19) 0.95544(17) 1.13869(15) 0.0678(4) Uani 1 1 d . . . . .
N6 N 0.60808(19) 0.48995(17) 0.28162(14) 0.0656(4) Uani 1 1 d . . . . .
N5 N 0.49788(18) 0.51753(17) 0.33320(15) 0.0658(4) Uani 1 1 d . . . . .
N4 N 0.68358(18) 0.33118(16) 0.40839(15) 0.0655(4) Uani 1 1 d . . . . .
N12 N 0.80012(18) 0.86659(16) 1.12901(15) 0.0642(4) Uani 1 1 d . . . . .
N9 N 0.97853(18) 0.81483(17) 0.94863(16) 0.0673(4) Uani 1 1 d . . . . .
N3 N 0.58790(19) 0.33707(17) 0.48108(15) 0.0672(4) Uani 1 1 d . . . . .
C14 C 0.5873(2) 0.9308(3) 0.88533(19) 0.0751(6) Uani 1 1 d . . . . .
C13 C 0.6093(3) 1.0368(3) 0.8313(2) 0.0884(7) Uani 1 1 d . . . . .
H13 H 0.545914 1.071868 0.785487 0.106 Uiso 1 1 calc R U . . .
C12 C 0.7432(3) 1.0823(2) 0.8575(2) 0.0787(6) Uani 1 1 d . . . . .
C4 C 0.5692(3) 0.2244(2) 0.5183(2) 0.0835(7) Uani 1 1 d . . . . .
H4 H 0.509304 0.202033 0.569645 0.100 Uiso 1 1 calc R U . . .
C6 C 0.7206(3) 0.2150(2) 0.4010(2) 0.0837(7) Uani 1 1 d . . . . .
H6 H 0.783458 0.187140 0.356096 0.100 Uiso 1 1 calc R U . . .
C17 C 0.8701(3) 0.6271(2) 0.9308(2) 0.0814(7) Uani 1 1 d . . . . .
H17 H 0.803020 0.561985 0.933646 0.098 Uiso 1 1 calc R U . . .
C5 C 0.6508(3) 0.1451(3) 0.4703(3) 0.0966(8) Uani 1 1 d . . . . .
H5 H 0.656755 0.061853 0.482552 0.116 Uiso 1 1 calc R U . . .
C3 C 0.9015(2) 0.6263(2) 0.45015(18) 0.0657(5) Uani 1 1 d . . . . .
C15 C 1.0568(3) 0.7370(3) 0.9034(2) 0.0839(7) Uani 1 1 d . . . . .
H15 H 1.142857 0.759832 0.882635 0.101 Uiso 1 1 calc R U . . .
C1 C 0.7669(2) 0.6833(2) 0.57471(18) 0.0687(5) Uani 1 1 d . . . . .
C2 C 0.8937(2) 0.7089(2) 0.5368(2) 0.0754(6) Uani 1 1 d . . . . .
H2 H 0.960586 0.770659 0.565221 0.091 Uiso 1 1 calc R U . . .
C16 C 0.9927(3) 0.6176(3) 0.8913(2) 0.0929(8) Uani 1 1 d . . . . .
H16 H 1.026004 0.546633 0.862609 0.112 Uiso 1 1 calc R U . . .
C18 C 0.9328(3) 0.9870(2) 1.2449(2) 0.0826(7) Uani 1 1 d . . . . .
H18 H 1.000399 1.047208 1.275091 0.099 Uiso 1 1 calc R U . . .
C7 C 0.4133(3) 0.5593(2) 0.2571(2) 0.0818(7) Uani 1 1 d . . . . .
H7 H 0.328857 0.584571 0.269484 0.098 Uiso 1 1 calc R U . . .
C20 C 0.7624(3) 0.8430(2) 1.2290(2) 0.0781(6) Uani 1 1 d . . . . .
H20 H 0.692175 0.785448 1.243963 0.094 Uiso 1 1 calc R U . . .
C9 C 0.5900(3) 0.5158(3) 0.17612(19) 0.0834(7) Uani 1 1 d . . . . .
H9 H 0.651340 0.505247 0.124150 0.100 Uiso 1 1 calc R U . . .
C19 C 0.8445(3) 0.9178(3) 1.3045(2) 0.0929(8) Uani 1 1 d . . . . .
H19 H 0.841915 0.921614 1.380120 0.112 Uiso 1 1 calc R U . . .
C21 C 0.8161(3) 1.1970(3) 0.8210(3) 0.1099(10) Uani 1 1 d . . . . .
H21A H 0.790626 1.268194 0.861180 0.165 Uiso 1 1 calc R U . . .
H21B H 0.792600 1.203460 0.744113 0.165 Uiso 1 1 calc R U . . .
H21C H 0.912134 1.193180 0.834182 0.165 Uiso 1 1 calc R U . . .
C8 C 0.4672(3) 0.5601(3) 0.1577(2) 0.0937(8) Uani 1 1 d . . . . .
H8 H 0.428046 0.585529 0.092033 0.112 Uiso 1 1 calc R U . . .
C22 C 0.4611(3) 0.8442(3) 0.8871(3) 0.1046(9) Uani 1 1 d . . . . .
H22A H 0.471005 0.767608 0.847030 0.157 Uiso 1 1 calc R U . . .
H22B H 0.385077 0.881348 0.853864 0.157 Uiso 1 1 calc R U . . .
H22C H 0.446415 0.828159 0.961536 0.157 Uiso 1 1 calc R U . . .
C10 C 0.7106(3) 0.7482(3) 0.6684(2) 0.0886(7) Uani 1 1 d . . . . .
H10A H 0.692983 0.830313 0.649584 0.133 Uiso 1 1 calc R U . . .
H10B H 0.775010 0.753264 0.731874 0.133 Uiso 1 1 calc R U . . .
H10C H 0.627766 0.702696 0.684038 0.133 Uiso 1 1 calc R U . . .
C11 C 1.0129(3) 0.6140(3) 0.3771(2) 0.0841(7) Uani 1 1 d . . . . .
H11A H 1.035207 0.529763 0.373849 0.126 Uiso 1 1 calc R U . . .
H11B H 1.091423 0.668018 0.405836 0.126 Uiso 1 1 calc R U . . .
H11C H 0.983629 0.636445 0.304877 0.126 Uiso 1 1 calc R U . . .
B1 B 0.7315(3) 0.4474(2) 0.3505(2) 0.0655(6) Uani 1 1 d . . . . .
B2 B 0.7455(3) 0.8088(2) 1.0144(2) 0.0655(6) Uani 1 1 d . . . . .
H1 H 0.808(2) 0.431(2) 0.2935(19) 0.072(6) Uiso 1 1 d . . . . .
H2A H 0.659(2) 0.737(2) 1.018(2) 0.077(7) Uiso 1 1 d . . . . .


_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 2.0955(17) . ?
Fe01 N1 2.0955(17) 2_666 ?
Fe01 N5 2.0644(18) 2_666 ?
Fe01 N5 2.0644(18) . ?
Fe01 N3 2.0545(18) . ?
Fe01 N3 2.0545(18) 2_666 ?
Fe02 N7 2.0951(18) 2_777 ?
Fe02 N7 2.0951(18) . ?
Fe02 N11 2.0630(19) . ?
Fe02 N11 2.0630(19) 2_777 ?
Fe02 N9 2.0585(18) 2_777 ?
Fe02 N9 2.0585(18) . ?
N7 N8 1.380(2) . ?
N7 C12 1.335(3) . ?
N2 N1 1.383(2) . ?
N2 C3 1.351(3) . ?
N2 B1 1.538(3) . ?
N10 N9 1.359(2) . ?
N10 C17 1.344(3) . ?
N10 B2 1.548(3) . ?
N8 C14 1.357(3) . ?
N8 B2 1.532(3) . ?
N1 C1 1.338(3) . ?
N11 N12 1.363(2) . ?
N11 C18 1.326(3) . ?
N6 N5 1.362(3) . ?
N6 C9 1.340(3) . ?
N6 B1 1.550(3) . ?
N5 C7 1.328(3) . ?
N4 N3 1.364(2) . ?
N4 C6 1.345(3) . ?
N4 B1 1.537(3) . ?
N12 C20 1.345(3) . ?
N12 B2 1.541(3) . ?
N9 C15 1.332(3) . ?
N3 C4 1.330(3) . ?
C14 C13 1.367(4) . ?
C14 C22 1.498(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.380(4) . ?
C12 C21 1.490(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.361(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.362(4) . ?
C5 H5 0.9300 . ?
C3 C2 1.366(3) . ?
C3 C11 1.496(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.383(4) . ?
C1 C2 1.391(3) . ?
C1 C10 1.494(3) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.385(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.375(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.359(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.360(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.10(2) . ?
B2 H2A 1.11(2) . ?

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 180.0 2_666 . ?
N5 Fe01 N1 92.98(7) . 2_666 ?
N5 Fe01 N1 87.02(7) 2_666 2_666 ?
N5 Fe01 N1 87.02(7) . . ?
N5 Fe01 N1 92.98(7) 2_666 . ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 93.79(7) 2_666 . ?
N3 Fe01 N1 93.79(7) . 2_666 ?
N3 Fe01 N1 86.21(7) 2_666 2_666 ?
N3 Fe01 N1 86.21(7) . . ?
N3 Fe01 N5 90.91(7) 2_666 . ?
N3 Fe01 N5 89.09(7) 2_666 2_666 ?
N3 Fe01 N5 90.91(7) . 2_666 ?
N3 Fe01 N5 89.09(7) . . ?
N3 Fe01 N3 180.0 . 2_666 ?
N7 Fe02 N7 180.0 . 2_777 ?
N11 Fe02 N7 86.29(7) 2_777 2_777 ?
N11 Fe02 N7 93.71(7) . 2_777 ?
N11 Fe02 N7 86.29(7) . . ?
N11 Fe02 N7 93.71(7) 2_777 . ?
N11 Fe02 N11 180.0 2_777 . ?
N9 Fe02 N7 86.49(7) . . ?
N9 Fe02 N7 93.51(7) . 2_777 ?
N9 Fe02 N7 93.51(7) 2_777 . ?
N9 Fe02 N7 86.49(7) 2_777 2_777 ?
N9 Fe02 N11 90.79(7) 2_777 . ?
N9 Fe02 N11 89.21(7) . . ?
N9 Fe02 N11 90.79(7) . 2_777 ?
N9 Fe02 N11 89.21(7) 2_777 2_777 ?
N9 Fe02 N9 180.0 . 2_777 ?
N8 N7 Fe02 117.64(13) . . ?
C12 N7 Fe02 136.03(16) . . ?
C12 N7 N8 106.32(19) . . ?
N1 N2 B1 118.99(16) . . ?
C3 N2 N1 110.30(17) . . ?
C3 N2 B1 130.65(18) . . ?
N9 N10 B2 119.77(16) . . ?
C17 N10 N9 109.21(19) . . ?
C17 N10 B2 131.0(2) . . ?
N7 N8 B2 119.22(17) . . ?
C14 N8 N7 109.75(19) . . ?
C14 N8 B2 131.0(2) . . ?
N2 N1 Fe01 117.52(12) . . ?
C1 N1 Fe01 136.35(15) . . ?
C1 N1 N2 105.88(17) . . ?
N12 N11 Fe02 118.67(13) . . ?
C18 N11 Fe02 134.90(18) . . ?
C18 N11 N12 106.2(2) . . ?
N5 N6 B1 118.74(16) . . ?
C9 N6 N5 109.5(2) . . ?
C9 N6 B1 131.6(2) . . ?
N6 N5 Fe01 119.03(13) . . ?
C7 N5 Fe01 134.97(18) . . ?
C7 N5 N6 105.84(19) . . ?
N3 N4 B1 120.09(17) . . ?
C6 N4 N3 109.1(2) . . ?
C6 N4 B1 130.8(2) . . ?
N11 N12 B2 119.28(17) . . ?
C20 N12 N11 109.6(2) . . ?
C20 N12 B2 131.1(2) . . ?
N10 N9 Fe02 118.38(13) . . ?
C15 N9 Fe02 135.41(17) . . ?
C15 N9 N10 106.15(19) . . ?
N4 N3 Fe01 118.05(13) . . ?
C4 N3 Fe01 135.49(17) . . ?
C4 N3 N4 106.28(19) . . ?
N8 C14 C13 106.9(2) . . ?
N8 C14 C22 122.9(2) . . ?
C13 C14 C22 130.2(2) . . ?
C14 C13 H13 126.3 . . ?
C14 C13 C12 107.4(2) . . ?
C12 C13 H13 126.3 . . ?
N7 C12 C13 109.7(2) . . ?
N7 C12 C21 122.2(2) . . ?
C13 C12 C21 128.1(2) . . ?
N3 C4 H4 124.7 . . ?
N3 C4 C5 110.7(2) . . ?
C5 C4 H4 124.7 . . ?
N4 C6 H6 125.6 . . ?
N4 C6 C5 108.7(2) . . ?
C5 C6 H6 125.6 . . ?
N10 C17 H17 125.5 . . ?
N10 C17 C16 109.1(2) . . ?
C16 C17 H17 125.5 . . ?
C4 C5 H5 127.4 . . ?
C6 C5 C4 105.2(2) . . ?
C6 C5 H5 127.4 . . ?
N2 C3 C2 107.0(2) . . ?
N2 C3 C11 123.0(2) . . ?
C2 C3 C11 129.9(2) . . ?
N9 C15 H15 124.5 . . ?
N9 C15 C16 110.9(2) . . ?
C16 C15 H15 124.5 . . ?
N1 C1 C2 109.6(2) . . ?
N1 C1 C10 123.0(2) . . ?
C2 C1 C10 127.4(2) . . ?
C3 C2 C1 107.2(2) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C17 C16 C15 104.6(2) . . ?
C17 C16 H16 127.7 . . ?
C15 C16 H16 127.7 . . ?
N11 C18 H18 124.8 . . ?
N11 C18 C19 110.5(2) . . ?
C19 C18 H18 124.8 . . ?
N5 C7 H7 124.5 . . ?
N5 C7 C8 111.0(3) . . ?
C8 C7 H7 124.5 . . ?
N12 C20 H20 125.9 . . ?
N12 C20 C19 108.3(2) . . ?
C19 C20 H20 125.9 . . ?
N6 C9 H9 125.7 . . ?
N6 C9 C8 108.6(2) . . ?
C8 C9 H9 125.7 . . ?
C18 C19 H19 127.3 . . ?
C20 C19 C18 105.4(2) . . ?
C20 C19 H19 127.3 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.5 . . ?
C9 C8 C7 105.0(2) . . ?
C9 C8 H8 127.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 107.25(18) . . ?
N2 B1 H1 111.4(12) . . ?
N6 B1 H1 106.8(12) . . ?
N4 B1 N2 109.52(18) . . ?
N4 B1 N6 108.46(18) . . ?
N4 B1 H1 113.1(12) . . ?
N10 B2 H2A 107.8(13) . . ?
N8 B2 N10 108.35(17) . . ?
N8 B2 N12 108.82(19) . . ?
N8 B2 H2A 111.7(13) . . ?
N12 B2 N10 107.80(18) . . ?
N12 B2 H2A 112.2(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -173.00(17) . . . . ?
Fe01 N1 C1 C10 6.8(4) . . . . ?
Fe01 N5 C7 C8 174.66(18) . . . . ?
Fe01 N3 C4 C5 174.4(2) . . . . ?
Fe02 N7 N8 C14 -178.95(15) . . . . ?
Fe02 N7 N8 B2 0.2(2) . . . . ?
Fe02 N7 C12 C13 178.18(19) . . . . ?
Fe02 N7 C12 C21 -2.1(4) . . . . ?
Fe02 N11 N12 C20 174.34(15) . . . . ?
Fe02 N11 N12 B2 -4.1(2) . . . . ?
Fe02 N11 C18 C19 -173.22(18) . . . . ?
Fe02 N9 C15 C16 176.37(19) . . . . ?
N7 N8 C14 C13 0.5(3) . . . . ?
N7 N8 C14 C22 -180.0(2) . . . . ?
N7 N8 B2 N10 -58.5(2) . . . . ?
N7 N8 B2 N12 58.5(2) . . . . ?
N2 N1 C1 C2 0.7(2) . . . . ?
N2 N1 C1 C10 -179.5(2) . . . . ?
N2 C3 C2 C1 -0.1(3) . . . . ?
N10 N9 C15 C16 -0.8(3) . . . . ?
N10 C17 C16 C15 -0.2(3) . . . . ?
N8 N7 C12 C13 -0.5(3) . . . . ?
N8 N7 C12 C21 179.2(3) . . . . ?
N8 C14 C13 C12 -0.8(3) . . . . ?
N1 N2 C3 C2 0.6(2) . . . . ?
N1 N2 C3 C11 -177.9(2) . . . . ?
N1 N2 B1 N6 62.0(2) . . . . ?
N1 N2 B1 N4 -55.6(2) . . . . ?
N1 C1 C2 C3 -0.4(3) . . . . ?
N11 N12 C20 C19 0.6(3) . . . . ?
N11 N12 B2 N10 60.5(2) . . . . ?
N11 N12 B2 N8 -56.8(2) . . . . ?
N11 C18 C19 C20 -0.7(3) . . . . ?
N6 N5 C7 C8 -0.5(3) . . . . ?
N6 C9 C8 C7 0.0(3) . . . . ?
N5 N6 C9 C8 -0.3(3) . . . . ?
N5 N6 B1 N2 -60.2(2) . . . . ?
N5 N6 B1 N4 58.0(2) . . . . ?
N5 C7 C8 C9 0.3(3) . . . . ?
N4 N3 C4 C5 -0.4(3) . . . . ?
N4 C6 C5 C4 0.7(3) . . . . ?
N12 N11 C18 C19 1.1(3) . . . . ?
N12 C20 C19 C18 0.0(3) . . . . ?
N9 N10 C17 C16 -0.3(3) . . . . ?
N9 N10 B2 N8 57.0(2) . . . . ?
N9 N10 B2 N12 -60.6(2) . . . . ?
N9 C15 C16 C17 0.6(3) . . . . ?
N3 N4 C6 C5 -1.0(3) . . . . ?
N3 N4 B1 N2 55.5(3) . . . . ?
N3 N4 B1 N6 -61.3(2) . . . . ?
N3 C4 C5 C6 -0.2(3) . . . . ?
C14 N8 B2 N10 120.5(2) . . . . ?
C14 N8 B2 N12 -122.6(2) . . . . ?
C14 C13 C12 N7 0.8(3) . . . . ?
C14 C13 C12 C21 -178.9(3) . . . . ?
C12 N7 N8 C14 0.0(3) . . . . ?
C12 N7 N8 B2 179.2(2) . . . . ?
C6 N4 N3 Fe01 -175.01(16) . . . . ?
C6 N4 N3 C4 0.8(3) . . . . ?
C6 N4 B1 N2 -124.4(2) . . . . ?
C6 N4 B1 N6 118.8(2) . . . . ?
C17 N10 N9 Fe02 -177.09(16) . . . . ?
C17 N10 N9 C15 0.6(3) . . . . ?
C17 N10 B2 N8 -121.9(3) . . . . ?
C17 N10 B2 N12 120.4(3) . . . . ?
C3 N2 N1 Fe01 174.31(13) . . . . ?
C3 N2 N1 C1 -0.8(2) . . . . ?
C3 N2 B1 N6 -115.0(2) . . . . ?
C3 N2 B1 N4 127.5(2) . . . . ?
C18 N11 N12 C20 -1.1(3) . . . . ?
C18 N11 N12 B2 -179.5(2) . . . . ?
C20 N12 B2 N10 -117.5(2) . . . . ?
C20 N12 B2 N8 125.2(2) . . . . ?
C9 N6 N5 Fe01 -175.60(15) . . . . ?
C9 N6 N5 C7 0.5(2) . . . . ?
C9 N6 B1 N2 113.6(3) . . . . ?
C9 N6 B1 N4 -128.2(2) . . . . ?
C22 C14 C13 C12 179.7(3) . . . . ?
C10 C1 C2 C3 179.8(2) . . . . ?
C11 C3 C2 C1 178.1(2) . . . . ?
B1 N2 N1 Fe01 -3.2(2) . . . . ?
B1 N2 N1 C1 -178.35(19) . . . . ?
B1 N2 C3 C2 177.8(2) . . . . ?
B1 N2 C3 C11 -0.7(4) . . . . ?
B1 N6 N5 Fe01 -0.5(2) . . . . ?
B1 N6 N5 C7 175.6(2) . . . . ?
B1 N6 C9 C8 -174.6(2) . . . . ?
B1 N4 N3 Fe01 5.1(2) . . . . ?
B1 N4 N3 C4 -179.1(2) . . . . ?
B1 N4 C6 C5 178.9(2) . . . . ?
B2 N10 N9 Fe02 3.8(2) . . . . ?
B2 N10 N9 C15 -178.5(2) . . . . ?
B2 N10 C17 C16 178.8(2) . . . . ?
B2 N8 C14 C13 -178.5(2) . . . . ?
B2 N8 C14 C22 1.0(4) . . . . ?
B2 N12 C20 C19 178.8(2) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_340K
_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_pr210_350kdown
_database_code_depnum_ccdc_archive 'CCDC 2261116'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9676(7)
_cell_length_b                   10.8692(8)
_cell_length_c                   12.2898(8)
_cell_angle_alpha                92.987(5)
_cell_angle_beta                 95.018(5)
_cell_angle_gamma                95.350(5)
_cell_volume                     1318.15(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5072
_cell_measurement_temperature    350(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.793
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9919
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.423
_diffrn_reflns_theta_min         3.518
_diffrn_ambient_temperature      350(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 3 sets of ω scans each set at different φ and/or 2θ angles and each scan (240.00 s exposure) covering 2.000\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4196
_reflns_number_total             5893
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5893
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.033
_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)+(0.0689P)²+0.1231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1294
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.05500(14) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.05696(14) Uani 1 2 d S . P . .
N7 N 0.80302(19) 1.00630(18) 0.92370(17) 0.0706(5) Uani 1 1 d . . . . .
N2 N 0.78320(18) 0.55303(17) 0.43628(15) 0.0636(4) Uani 1 1 d . . . . .
N10 N 0.8611(2) 0.74538(17) 0.96493(16) 0.0667(5) Uani 1 1 d . . . . .
N8 N 0.70587(19) 0.91241(18) 0.94143(16) 0.0677(5) Uani 1 1 d . . . . .
N1 N 0.69883(19) 0.58888(17) 0.51307(15) 0.0646(5) Uani 1 1 d . . . . .
N11 N 0.9060(2) 0.95499(18) 1.13919(16) 0.0703(5) Uani 1 1 d . . . . .
N6 N 0.6089(2) 0.48968(18) 0.28129(15) 0.0676(5) Uani 1 1 d . . . . .
N5 N 0.49868(19) 0.51738(18) 0.33207(16) 0.0677(5) Uani 1 1 d . . . . .
N4 N 0.68427(19) 0.33143(18) 0.40798(16) 0.0678(5) Uani 1 1 d . . . . .
N12 N 0.7993(2) 0.86617(17) 1.12896(16) 0.0669(5) Uani 1 1 d . . . . .
N9 N 0.9780(2) 0.81379(18) 0.94860(17) 0.0700(5) Uani 1 1 d . . . . .
N3 N 0.5891(2) 0.33676(18) 0.48104(16) 0.0693(5) Uani 1 1 d . . . . .
C14 C 0.5871(2) 0.9302(3) 0.8853(2) 0.0765(7) Uani 1 1 d . . . . .
C13 C 0.6077(3) 1.0354(3) 0.8309(2) 0.0913(8) Uani 1 1 d . . . . .
H13 H 0.544014 1.069819 0.785027 0.110 Uiso 1 1 calc R U . . .
C12 C 0.7417(3) 1.0813(3) 0.8570(2) 0.0812(7) Uani 1 1 d . . . . .
C4 C 0.5712(3) 0.2239(2) 0.5176(2) 0.0863(7) Uani 1 1 d . . . . .
H4 H 0.511922 0.201150 0.569035 0.104 Uiso 1 1 calc R U . . .
C6 C 0.7217(3) 0.2155(3) 0.4002(3) 0.0861(8) Uani 1 1 d . . . . .
H6 H 0.784577 0.188025 0.355344 0.103 Uiso 1 1 calc R U . . .
C17 C 0.8694(3) 0.6274(2) 0.9316(2) 0.0848(7) Uani 1 1 d . . . . .
H17 H 0.802388 0.562572 0.935057 0.102 Uiso 1 1 calc R U . . .
C5 C 0.6518(3) 0.1452(3) 0.4693(3) 0.0997(9) Uani 1 1 d . . . . .
H5 H 0.657542 0.061980 0.481111 0.120 Uiso 1 1 calc R U . . .
C3 C 0.9017(2) 0.6261(2) 0.4493(2) 0.0682(6) Uani 1 1 d . . . . .
C15 C 1.0557(3) 0.7355(3) 0.9036(2) 0.0861(7) Uani 1 1 d . . . . .
H15 H 1.141774 0.757784 0.883034 0.103 Uiso 1 1 calc R U . . .
C1 C 0.7683(3) 0.6835(2) 0.5741(2) 0.0712(6) Uani 1 1 d . . . . .
C2 C 0.8941(3) 0.7087(2) 0.5360(2) 0.0770(6) Uani 1 1 d . . . . .
H2 H 0.961046 0.770320 0.564087 0.092 Uiso 1 1 calc R U . . .
C16 C 0.9914(4) 0.6170(3) 0.8917(3) 0.0967(9) Uani 1 1 d . . . . .
H16 H 1.023917 0.546014 0.862830 0.116 Uiso 1 1 calc R U . . .
C18 C 0.9305(3) 0.9857(3) 1.2455(2) 0.0861(8) Uani 1 1 d . . . . .
H18 H 0.997719 1.045680 1.276169 0.103 Uiso 1 1 calc R U . . .
C7 C 0.4141(3) 0.5590(3) 0.2557(2) 0.0844(7) Uani 1 1 d . . . . .
H7 H 0.329688 0.584206 0.267596 0.101 Uiso 1 1 calc R U . . .
C20 C 0.7617(3) 0.8424(3) 1.2285(2) 0.0804(7) Uani 1 1 d . . . . .
H20 H 0.691796 0.784599 1.243261 0.096 Uiso 1 1 calc R U . . .
C9 C 0.5916(3) 0.5155(3) 0.1760(2) 0.0850(8) Uani 1 1 d . . . . .
H9 H 0.653384 0.505076 0.124614 0.102 Uiso 1 1 calc R U . . .
C19 C 0.8429(4) 0.9167(3) 1.3040(2) 0.0959(9) Uani 1 1 d . . . . .
H19 H 0.839864 0.920280 1.379516 0.115 Uiso 1 1 calc R U . . .
C21 C 0.8138(4) 1.1954(3) 0.8203(3) 0.1137(12) Uani 1 1 d . . . . .
H21A H 0.787451 1.266498 0.859697 0.170 Uiso 1 1 calc R U . . .
H21B H 0.790942 1.201191 0.743337 0.170 Uiso 1 1 calc R U . . .
H21C H 0.909705 1.192307 0.834146 0.170 Uiso 1 1 calc R U . . .
C8 C 0.4692(3) 0.5595(3) 0.1562(2) 0.0968(9) Uani 1 1 d . . . . .
H8 H 0.430791 0.584476 0.090304 0.116 Uiso 1 1 calc R U . . .
C22 C 0.4611(3) 0.8438(4) 0.8876(3) 0.1076(10) Uani 1 1 d . . . . .
H22A H 0.474059 0.764590 0.853999 0.161 Uiso 1 1 calc R U . . .
H22B H 0.386669 0.877145 0.848110 0.161 Uiso 1 1 calc R U . . .
H22C H 0.441773 0.834442 0.962018 0.161 Uiso 1 1 calc R U . . .
C10 C 0.7119(3) 0.7482(3) 0.6677(2) 0.0916(8) Uani 1 1 d . . . . .
H10A H 0.700328 0.832052 0.650957 0.137 Uiso 1 1 calc R U . . .
H10B H 0.773214 0.748021 0.732481 0.137 Uiso 1 1 calc R U . . .
H10C H 0.625995 0.706083 0.679879 0.137 Uiso 1 1 calc R U . . .
C11 C 1.0129(3) 0.6132(3) 0.3763(2) 0.0870(7) Uani 1 1 d . . . . .
H11A H 1.035462 0.529218 0.373730 0.131 Uiso 1 1 calc R U . . .
H11B H 1.091233 0.667476 0.404352 0.131 Uiso 1 1 calc R U . . .
H11C H 0.983407 0.634739 0.303864 0.131 Uiso 1 1 calc R U . . .
B1 B 0.7319(3) 0.4474(3) 0.3505(2) 0.0678(6) Uani 1 1 d . . . . .
B2 B 0.7456(3) 0.8085(3) 1.0141(2) 0.0677(6) Uani 1 1 d . . . . .
H1 H 0.806(2) 0.430(2) 0.294(2) 0.077(7) Uiso 1 1 d . . . . .
H2A H 0.658(3) 0.740(2) 1.018(2) 0.080(7) Uiso 1 1 d . . . . .


_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 2.1114(19) 2_666 ?
Fe01 N1 2.1114(19) . ?
Fe01 N5 2.0813(19) 2_666 ?
Fe01 N5 2.0813(19) . ?
Fe01 N3 2.068(2) 2_666 ?
Fe01 N3 2.068(2) . ?
Fe02 N7 2.109(2) 2_777 ?
Fe02 N7 2.109(2) . ?
Fe02 N11 2.080(2) 2_777 ?
Fe02 N11 2.080(2) . ?
Fe02 N9 2.074(2) 2_777 ?
Fe02 N9 2.074(2) . ?
N7 N8 1.379(3) . ?
N7 C12 1.336(3) . ?
N2 N1 1.383(3) . ?
N2 C3 1.353(3) . ?
N2 B1 1.536(3) . ?
N10 N9 1.359(3) . ?
N10 C17 1.338(3) . ?
N10 B2 1.545(3) . ?
N8 C14 1.352(3) . ?
N8 B2 1.535(3) . ?
N1 C1 1.340(3) . ?
N11 N12 1.361(3) . ?
N11 C18 1.327(3) . ?
N6 N5 1.360(3) . ?
N6 C9 1.338(3) . ?
N6 B1 1.550(4) . ?
N5 C7 1.331(3) . ?
N4 N3 1.365(3) . ?
N4 C6 1.348(3) . ?
N4 B1 1.533(4) . ?
N12 C20 1.342(3) . ?
N12 B2 1.544(4) . ?
N9 C15 1.333(3) . ?
N3 C4 1.330(3) . ?
C14 C13 1.363(4) . ?
C14 C22 1.500(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.385(4) . ?
C12 C21 1.486(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.374(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.364(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.362(4) . ?
C5 H5 0.9300 . ?
C3 C2 1.368(4) . ?
C3 C11 1.499(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.378(4) . ?
C1 C2 1.386(3) . ?
C1 C10 1.496(4) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.373(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.383(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.355(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.358(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.08(2) . ?
B2 H2A 1.10(3) . ?

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 180.0 . 2_666 ?
N5 Fe01 N1 86.72(7) . . ?
N5 Fe01 N1 93.28(7) 2_666 . ?
N5 Fe01 N1 93.28(7) . 2_666 ?
N5 Fe01 N1 86.72(7) 2_666 2_666 ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 94.08(8) . 2_666 ?
N3 Fe01 N1 94.08(8) 2_666 . ?
N3 Fe01 N1 85.92(8) . . ?
N3 Fe01 N1 85.92(8) 2_666 2_666 ?
N3 Fe01 N5 88.83(8) . . ?
N3 Fe01 N5 91.17(8) . 2_666 ?
N3 Fe01 N5 88.83(8) 2_666 2_666 ?
N3 Fe01 N5 91.17(8) 2_666 . ?
N3 Fe01 N3 180.0 2_666 . ?
N7 Fe02 N7 180.00(11) . 2_777 ?
N11 Fe02 N7 93.99(8) . 2_777 ?
N11 Fe02 N7 86.01(8) 2_777 2_777 ?
N11 Fe02 N7 93.99(8) 2_777 . ?
N11 Fe02 N7 86.01(8) . . ?
N11 Fe02 N11 180.00(10) . 2_777 ?
N9 Fe02 N7 86.18(8) . . ?
N9 Fe02 N7 93.82(8) . 2_777 ?
N9 Fe02 N7 93.82(8) 2_777 . ?
N9 Fe02 N7 86.18(8) 2_777 2_777 ?
N9 Fe02 N11 89.03(8) 2_777 2_777 ?
N9 Fe02 N11 90.97(8) . 2_777 ?
N9 Fe02 N11 89.03(8) . . ?
N9 Fe02 N11 90.97(8) 2_777 . ?
N9 Fe02 N9 180.0 . 2_777 ?
N8 N7 Fe02 117.73(13) . . ?
C12 N7 Fe02 136.07(18) . . ?
C12 N7 N8 106.2(2) . . ?
N1 N2 B1 119.34(17) . . ?
C3 N2 N1 110.04(19) . . ?
C3 N2 B1 130.6(2) . . ?
N9 N10 B2 119.89(18) . . ?
C17 N10 N9 109.1(2) . . ?
C17 N10 B2 131.0(2) . . ?
N7 N8 B2 119.05(18) . . ?
C14 N8 N7 109.7(2) . . ?
C14 N8 B2 131.2(2) . . ?
N2 N1 Fe01 117.27(13) . . ?
C1 N1 Fe01 136.37(16) . . ?
C1 N1 N2 106.11(18) . . ?
N12 N11 Fe02 118.55(15) . . ?
C18 N11 Fe02 135.2(2) . . ?
C18 N11 N12 106.0(2) . . ?
N5 N6 B1 118.92(18) . . ?
C9 N6 N5 109.4(2) . . ?
C9 N6 B1 131.5(2) . . ?
N6 N5 Fe01 118.91(14) . . ?
C7 N5 Fe01 134.83(19) . . ?
C7 N5 N6 106.1(2) . . ?
N3 N4 B1 120.26(18) . . ?
C6 N4 N3 109.1(2) . . ?
C6 N4 B1 130.6(2) . . ?
N11 N12 B2 119.34(18) . . ?
C20 N12 N11 109.3(2) . . ?
C20 N12 B2 131.3(2) . . ?
N10 N9 Fe02 118.26(14) . . ?
C15 N9 Fe02 135.63(18) . . ?
C15 N9 N10 106.1(2) . . ?
N4 N3 Fe01 117.91(14) . . ?
C4 N3 Fe01 135.86(18) . . ?
C4 N3 N4 106.0(2) . . ?
N8 C14 C13 107.4(2) . . ?
N8 C14 C22 122.8(3) . . ?
C13 C14 C22 129.7(3) . . ?
C14 C13 H13 126.5 . . ?
C14 C13 C12 106.9(2) . . ?
C12 C13 H13 126.5 . . ?
N7 C12 C13 109.7(2) . . ?
N7 C12 C21 122.2(3) . . ?
C13 C12 C21 128.1(3) . . ?
N3 C4 H4 124.4 . . ?
N3 C4 C5 111.1(3) . . ?
C5 C4 H4 124.4 . . ?
N4 C6 H6 125.7 . . ?
N4 C6 C5 108.6(3) . . ?
C5 C6 H6 125.7 . . ?
N10 C17 H17 125.3 . . ?
N10 C17 C16 109.4(2) . . ?
C16 C17 H17 125.3 . . ?
C4 C5 H5 127.4 . . ?
C6 C5 C4 105.2(3) . . ?
C6 C5 H5 127.4 . . ?
N2 C3 C2 107.0(2) . . ?
N2 C3 C11 123.0(2) . . ?
C2 C3 C11 130.0(2) . . ?
N9 C15 H15 124.5 . . ?
N9 C15 C16 111.0(3) . . ?
C16 C15 H15 124.5 . . ?
N1 C1 C2 109.6(2) . . ?
N1 C1 C10 122.7(2) . . ?
C2 C1 C10 127.7(2) . . ?
C3 C2 C1 107.3(2) . . ?
C3 C2 H2 126.3 . . ?
C1 C2 H2 126.3 . . ?
C17 C16 C15 104.5(3) . . ?
C17 C16 H16 127.8 . . ?
C15 C16 H16 127.8 . . ?
N11 C18 H18 124.7 . . ?
N11 C18 C19 110.7(3) . . ?
C19 C18 H18 124.7 . . ?
N5 C7 H7 124.7 . . ?
N5 C7 C8 110.6(3) . . ?
C8 C7 H7 124.7 . . ?
N12 C20 H20 125.8 . . ?
N12 C20 C19 108.5(3) . . ?
C19 C20 H20 125.8 . . ?
N6 C9 H9 125.5 . . ?
N6 C9 C8 109.0(3) . . ?
C8 C9 H9 125.5 . . ?
C18 C19 H19 127.3 . . ?
C20 C19 C18 105.5(2) . . ?
C20 C19 H19 127.3 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.6 . . ?
C9 C8 C7 104.9(2) . . ?
C9 C8 H8 127.6 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 107.3(2) . . ?
N2 B1 H1 112.3(13) . . ?
N6 B1 H1 106.2(13) . . ?
N4 B1 N2 109.8(2) . . ?
N4 B1 N6 108.5(2) . . ?
N4 B1 H1 112.5(13) . . ?
N10 B2 H2A 109.5(14) . . ?
N8 B2 N10 108.79(19) . . ?
N8 B2 N12 108.7(2) . . ?
N8 B2 H2A 110.2(14) . . ?
N12 B2 N10 108.1(2) . . ?
N12 B2 H2A 111.4(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -172.94(18) . . . . ?
Fe01 N1 C1 C10 6.7(4) . . . . ?
Fe01 N5 C7 C8 174.71(19) . . . . ?
Fe01 N3 C4 C5 173.8(2) . . . . ?
Fe02 N7 N8 C14 -179.04(16) . . . . ?
Fe02 N7 N8 B2 -0.5(3) . . . . ?
Fe02 N7 C12 C13 178.4(2) . . . . ?
Fe02 N7 C12 C21 -1.7(4) . . . . ?
Fe02 N11 N12 C20 174.05(16) . . . . ?
Fe02 N11 N12 B2 -4.1(3) . . . . ?
Fe02 N11 C18 C19 -172.9(2) . . . . ?
Fe02 N9 C15 C16 176.5(2) . . . . ?
N7 N8 C14 C13 0.2(3) . . . . ?
N7 N8 C14 C22 -180.0(2) . . . . ?
N7 N8 B2 N10 -58.2(3) . . . . ?
N7 N8 B2 N12 59.4(3) . . . . ?
N2 N1 C1 C2 0.8(3) . . . . ?
N2 N1 C1 C10 -179.5(2) . . . . ?
N2 C3 C2 C1 -0.2(3) . . . . ?
N10 N9 C15 C16 -0.7(3) . . . . ?
N10 C17 C16 C15 0.3(3) . . . . ?
N8 N7 C12 C13 -0.9(3) . . . . ?
N8 N7 C12 C21 179.0(3) . . . . ?
N8 C14 C13 C12 -0.8(3) . . . . ?
N1 N2 C3 C2 0.7(3) . . . . ?
N1 N2 C3 C11 -178.0(2) . . . . ?
N1 N2 B1 N6 62.1(3) . . . . ?
N1 N2 B1 N4 -55.6(3) . . . . ?
N1 C1 C2 C3 -0.4(3) . . . . ?
N11 N12 C20 C19 0.7(3) . . . . ?
N11 N12 B2 N10 60.8(3) . . . . ?
N11 N12 B2 N8 -57.2(3) . . . . ?
N11 C18 C19 C20 -0.6(3) . . . . ?
N6 N5 C7 C8 -0.5(3) . . . . ?
N6 C9 C8 C7 0.2(3) . . . . ?
N5 N6 C9 C8 -0.5(3) . . . . ?
N5 N6 B1 N2 -60.3(3) . . . . ?
N5 N6 B1 N4 58.3(3) . . . . ?
N5 C7 C8 C9 0.2(3) . . . . ?
N4 N3 C4 C5 -0.5(3) . . . . ?
N4 C6 C5 C4 0.3(4) . . . . ?
N12 N11 C18 C19 1.0(3) . . . . ?
N12 C20 C19 C18 -0.1(3) . . . . ?
N9 N10 C17 C16 -0.7(3) . . . . ?
N9 N10 B2 N8 57.2(3) . . . . ?
N9 N10 B2 N12 -60.7(3) . . . . ?
N9 C15 C16 C17 0.2(4) . . . . ?
N3 N4 C6 C5 -0.6(3) . . . . ?
N3 N4 B1 N2 55.2(3) . . . . ?
N3 N4 B1 N6 -61.8(3) . . . . ?
N3 C4 C5 C6 0.1(4) . . . . ?
C14 N8 B2 N10 120.0(3) . . . . ?
C14 N8 B2 N12 -122.5(3) . . . . ?
C14 C13 C12 N7 1.0(3) . . . . ?
C14 C13 C12 C21 -178.8(3) . . . . ?
C12 N7 N8 C14 0.4(3) . . . . ?
C12 N7 N8 B2 178.9(2) . . . . ?
C6 N4 N3 Fe01 -174.77(17) . . . . ?
C6 N4 N3 C4 0.7(3) . . . . ?
C6 N4 B1 N2 -124.4(3) . . . . ?
C6 N4 B1 N6 118.6(3) . . . . ?
C17 N10 N9 Fe02 -176.88(17) . . . . ?
C17 N10 N9 C15 0.8(3) . . . . ?
C17 N10 B2 N8 -122.1(3) . . . . ?
C17 N10 B2 N12 120.0(3) . . . . ?
C3 N2 N1 Fe01 174.22(14) . . . . ?
C3 N2 N1 C1 -0.9(3) . . . . ?
C3 N2 B1 N6 -114.7(2) . . . . ?
C3 N2 B1 N4 127.5(2) . . . . ?
C18 N11 N12 C20 -1.1(3) . . . . ?
C18 N11 N12 B2 -179.3(2) . . . . ?
C20 N12 B2 N10 -117.0(3) . . . . ?
C20 N12 B2 N8 125.1(3) . . . . ?
C9 N6 N5 Fe01 -175.50(16) . . . . ?
C9 N6 N5 C7 0.7(3) . . . . ?
C9 N6 B1 N2 113.3(3) . . . . ?
C9 N6 B1 N4 -128.1(3) . . . . ?
C22 C14 C13 C12 179.5(3) . . . . ?
C10 C1 C2 C3 179.9(3) . . . . ?
C11 C3 C2 C1 178.4(3) . . . . ?
B1 N2 N1 Fe01 -3.3(3) . . . . ?
B1 N2 N1 C1 -178.4(2) . . . . ?
B1 N2 C3 C2 177.8(2) . . . . ?
B1 N2 C3 C11 -0.9(4) . . . . ?
B1 N6 N5 Fe01 -0.6(3) . . . . ?
B1 N6 N5 C7 175.6(2) . . . . ?
B1 N6 C9 C8 -174.6(2) . . . . ?
B1 N4 N3 Fe01 5.6(3) . . . . ?
B1 N4 N3 C4 -179.0(2) . . . . ?
B1 N4 C6 C5 179.0(3) . . . . ?
B2 N10 N9 Fe02 3.7(3) . . . . ?
B2 N10 N9 C15 -178.6(2) . . . . ?
B2 N10 C17 C16 178.6(3) . . . . ?
B2 N8 C14 C13 -178.0(2) . . . . ?
B2 N8 C14 C22 1.8(4) . . . . ?
B2 N12 C20 C19 178.6(3) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_350Kdown
_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_pr210_360k
_database_code_depnum_ccdc_archive 'CCDC 2261117'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9836(4)
_cell_length_b                   10.9033(5)
_cell_length_c                   12.2973(5)
_cell_angle_alpha                93.054(3)
_cell_angle_beta                 95.025(3)
_cell_angle_gamma                95.275(3)
_cell_volume                     1325.28(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5898
_cell_measurement_temperature    360(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.794
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11250
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         3.089
_diffrn_ambient_temperature      360(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 6 sets of ω scans each set at different φ and/or
 2θ angles and each scan (240.00 s exposure) covering 2.000\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4414
_reflns_number_total             6022
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.044
_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)+(0.0652P)²+0.2267P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1260
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.05760(13) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.05977(13) Uani 1 2 d S . P . .
N7 N 0.80181(19) 1.00600(18) 0.92330(17) 0.0736(5) Uani 1 1 d . . . . .
N2 N 0.78376(18) 0.55317(17) 0.43599(15) 0.0666(4) Uani 1 1 d . . . . .
N10 N 0.86086(19) 0.74549(16) 0.96504(16) 0.0686(4) Uani 1 1 d . . . . .
N8 N 0.70548(18) 0.91182(18) 0.94109(16) 0.0700(5) Uani 1 1 d . . . . .
N1 N 0.69961(19) 0.58900(17) 0.51273(15) 0.0678(4) Uani 1 1 d . . . . .
N11 N 0.9049(2) 0.95480(18) 1.13957(16) 0.0733(5) Uani 1 1 d . . . . .
N6 N 0.6095(2) 0.48991(18) 0.28088(15) 0.0703(5) Uani 1 1 d . . . . .
N5 N 0.49895(19) 0.51704(18) 0.33106(15) 0.0712(5) Uani 1 1 d . . . . .
N4 N 0.68546(19) 0.33212(18) 0.40771(16) 0.0709(5) Uani 1 1 d . . . . .
N12 N 0.79875(19) 0.86620(17) 1.12890(16) 0.0689(4) Uani 1 1 d . . . . .
N9 N 0.97750(19) 0.81313(18) 0.94846(17) 0.0736(5) Uani 1 1 d . . . . .
N3 N 0.5904(2) 0.33660(18) 0.48075(16) 0.0727(5) Uani 1 1 d . . . . .
C14 C 0.5863(2) 0.9294(3) 0.8853(2) 0.0802(7) Uani 1 1 d . . . . .
C13 C 0.6065(3) 1.0338(3) 0.8308(2) 0.0950(8) Uani 1 1 d . . . . .
H13 H 0.542578 1.067907 0.784968 0.114 Uiso 1 1 calc R U . . .
C12 C 0.7403(3) 1.0800(3) 0.8563(2) 0.0844(7) Uani 1 1 d . . . . .
C4 C 0.5730(3) 0.2240(3) 0.5168(3) 0.0910(8) Uani 1 1 d . . . . .
H4 H 0.513816 0.201053 0.568146 0.109 Uiso 1 1 calc R U . . .
C6 C 0.7228(3) 0.2165(3) 0.3998(3) 0.0905(8) Uani 1 1 d . . . . .
H6 H 0.785544 0.189407 0.354671 0.109 Uiso 1 1 calc R U . . .
C17 C 0.8684(3) 0.6276(2) 0.9316(2) 0.0879(7) Uani 1 1 d . . . . .
H17 H 0.801262 0.563264 0.935039 0.105 Uiso 1 1 calc R U . . .
C5 C 0.6540(4) 0.1458(3) 0.4682(3) 0.1045(9) Uani 1 1 d . . . . .
H5 H 0.660206 0.062769 0.479625 0.125 Uiso 1 1 calc R U . . .
C3 C 0.9021(2) 0.6256(2) 0.4486(2) 0.0712(5) Uani 1 1 d . . . . .
C15 C 1.0546(3) 0.7344(3) 0.9037(2) 0.0899(7) Uani 1 1 d . . . . .
H15 H 1.140619 0.756072 0.883144 0.108 Uiso 1 1 calc R U . . .
C1 C 0.7691(3) 0.6837(2) 0.57332(19) 0.0735(6) Uani 1 1 d . . . . .
C2 C 0.8947(3) 0.7083(2) 0.5350(2) 0.0806(6) Uani 1 1 d . . . . .
H2 H 0.961579 0.769703 0.562855 0.097 Uiso 1 1 calc R U . . .
C16 C 0.9899(4) 0.6169(3) 0.8919(3) 0.1007(9) Uani 1 1 d . . . . .
H16 H 1.022151 0.545854 0.863105 0.121 Uiso 1 1 calc R U . . .
C18 C 0.9285(3) 0.9845(3) 1.2460(2) 0.0890(7) Uani 1 1 d . . . . .
H18 H 0.995342 1.044143 1.277270 0.107 Uiso 1 1 calc R U . . .
C7 C 0.4153(3) 0.5585(3) 0.2543(2) 0.0870(7) Uani 1 1 d . . . . .
H7 H 0.330866 0.583713 0.265821 0.104 Uiso 1 1 calc R U . . .
C20 C 0.7603(3) 0.8417(3) 1.2279(2) 0.0838(7) Uani 1 1 d . . . . .
H20 H 0.690285 0.783993 1.241940 0.101 Uiso 1 1 calc R U . . .
C9 C 0.5929(3) 0.5157(3) 0.1757(2) 0.0888(8) Uani 1 1 d . . . . .
H9 H 0.655042 0.505588 0.124698 0.107 Uiso 1 1 calc R U . . .
C19 C 0.8407(4) 0.9152(3) 1.3040(2) 0.0983(9) Uani 1 1 d . . . . .
H19 H 0.837370 0.918283 1.379411 0.118 Uiso 1 1 calc R U . . .
C21 C 0.8123(4) 1.1937(3) 0.8192(3) 0.1189(12) Uani 1 1 d . . . . .
H21A H 0.782664 1.264911 0.855818 0.178 Uiso 1 1 calc R U . . .
H21B H 0.792852 1.197024 0.741646 0.178 Uiso 1 1 calc R U . . .
H21C H 0.907856 1.192473 0.836280 0.178 Uiso 1 1 calc R U . . .
C8 C 0.4704(3) 0.5592(3) 0.1555(2) 0.0995(9) Uani 1 1 d . . . . .
H8 H 0.432199 0.583985 0.089497 0.119 Uiso 1 1 calc R U . . .
C22 C 0.4607(3) 0.8433(4) 0.8878(3) 0.1135(11) Uani 1 1 d . . . . .
H22A H 0.471516 0.766089 0.849844 0.170 Uiso 1 1 calc R U . . .
H22B H 0.385127 0.879032 0.852741 0.170 Uiso 1 1 calc R U . . .
H22C H 0.445064 0.829667 0.962282 0.170 Uiso 1 1 calc R U . . .
C10 C 0.7129(3) 0.7481(3) 0.6667(2) 0.0957(8) Uani 1 1 d . . . . .
H10A H 0.693958 0.829334 0.647532 0.144 Uiso 1 1 calc R U . . .
H10B H 0.777435 0.754085 0.729797 0.144 Uiso 1 1 calc R U . . .
H10C H 0.630979 0.702153 0.682780 0.144 Uiso 1 1 calc R U . . .
C11 C 1.0131(3) 0.6127(3) 0.3757(2) 0.0916(8) Uani 1 1 d . . . . .
H11A H 1.035358 0.528825 0.372889 0.137 Uiso 1 1 calc R U . . .
H11B H 1.091357 0.666445 0.404001 0.137 Uiso 1 1 calc R U . . .
H11C H 0.983794 0.634428 0.303408 0.137 Uiso 1 1 calc R U . . .
B1 B 0.7322(3) 0.4477(3) 0.3504(2) 0.0714(6) Uani 1 1 d . . . . .
B2 B 0.7452(3) 0.8092(3) 1.0139(2) 0.0706(6) Uani 1 1 d . . . . .
H1 H 0.805(2) 0.428(2) 0.294(2) 0.077(7) Uiso 1 1 d . . . . .
H2A H 0.658(3) 0.738(2) 1.018(2) 0.085(7) Uiso 1 1 d . . . . .


_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 2.1239(19) . ?
Fe01 N1 2.1239(19) 2_666 ?
Fe01 N5 2.0948(19) . ?
Fe01 N5 2.0948(19) 2_666 ?
Fe01 N3 2.082(2) 2_666 ?
Fe01 N3 2.082(2) . ?
Fe02 N7 2.1242(19) . ?
Fe02 N7 2.1242(19) 2_777 ?
Fe02 N11 2.093(2) 2_777 ?
Fe02 N11 2.093(2) . ?
Fe02 N9 2.087(2) . ?
Fe02 N9 2.087(2) 2_777 ?
N7 N8 1.381(3) . ?
N7 C12 1.334(3) . ?
N2 N1 1.382(2) . ?
N2 C3 1.352(3) . ?
N2 B1 1.537(3) . ?
N10 N9 1.357(3) . ?
N10 C17 1.340(3) . ?
N10 B2 1.550(3) . ?
N8 C14 1.355(3) . ?
N8 B2 1.529(3) . ?
N1 C1 1.341(3) . ?
N11 N12 1.359(3) . ?
N11 C18 1.327(3) . ?
N6 N5 1.359(3) . ?
N6 C9 1.337(3) . ?
N6 B1 1.551(3) . ?
N5 C7 1.331(3) . ?
N4 N3 1.365(3) . ?
N4 C6 1.348(3) . ?
N4 B1 1.531(4) . ?
N12 C20 1.342(3) . ?
N12 B2 1.544(3) . ?
N9 C15 1.333(3) . ?
N3 C4 1.329(3) . ?
C14 C13 1.361(4) . ?
C14 C22 1.499(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.387(4) . ?
C12 C21 1.488(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.359(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.359(4) . ?
C5 H5 0.9300 . ?
C3 C2 1.367(4) . ?
C3 C11 1.497(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.375(4) . ?
C1 C2 1.386(3) . ?
C1 C10 1.492(4) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.375(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.377(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.354(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.359(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.08(2) . ?
B2 H2A 1.12(3) . ?

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 180.0 2_666 . ?
N5 Fe01 N1 86.52(7) 2_666 2_666 ?
N5 Fe01 N1 93.48(7) . 2_666 ?
N5 Fe01 N1 93.48(7) 2_666 . ?
N5 Fe01 N1 86.52(7) . . ?
N5 Fe01 N5 180.0 2_666 . ?
N3 Fe01 N1 85.65(7) . . ?
N3 Fe01 N1 85.65(7) 2_666 2_666 ?
N3 Fe01 N1 94.35(7) . 2_666 ?
N3 Fe01 N1 94.35(7) 2_666 . ?
N3 Fe01 N5 91.36(8) . 2_666 ?
N3 Fe01 N5 88.64(8) . . ?
N3 Fe01 N5 91.36(8) 2_666 . ?
N3 Fe01 N5 88.64(8) 2_666 2_666 ?
N3 Fe01 N3 180.0 2_666 . ?
N7 Fe02 N7 180.0 2_777 . ?
N11 Fe02 N7 85.72(8) . . ?
N11 Fe02 N7 94.28(8) 2_777 . ?
N11 Fe02 N7 85.72(8) 2_777 2_777 ?
N11 Fe02 N7 94.28(8) . 2_777 ?
N11 Fe02 N11 180.00(5) . 2_777 ?
N9 Fe02 N7 85.97(8) 2_777 2_777 ?
N9 Fe02 N7 94.02(8) 2_777 . ?
N9 Fe02 N7 94.03(8) . 2_777 ?
N9 Fe02 N7 85.98(8) . . ?
N9 Fe02 N11 91.21(8) . 2_777 ?
N9 Fe02 N11 88.79(8) 2_777 2_777 ?
N9 Fe02 N11 91.21(8) 2_777 . ?
N9 Fe02 N11 88.79(8) . . ?
N9 Fe02 N9 180.0 2_777 . ?
N8 N7 Fe02 117.51(13) . . ?
C12 N7 Fe02 136.18(18) . . ?
C12 N7 N8 106.3(2) . . ?
N1 N2 B1 119.18(17) . . ?
C3 N2 N1 110.30(18) . . ?
C3 N2 B1 130.46(19) . . ?
N9 N10 B2 119.94(17) . . ?
C17 N10 N9 109.2(2) . . ?
C17 N10 B2 130.8(2) . . ?
N7 N8 B2 119.28(18) . . ?
C14 N8 N7 109.6(2) . . ?
C14 N8 B2 131.1(2) . . ?
N2 N1 Fe01 117.37(13) . . ?
C1 N1 Fe01 136.42(16) . . ?
C1 N1 N2 105.93(18) . . ?
N12 N11 Fe02 118.52(14) . . ?
C18 N11 Fe02 135.5(2) . . ?
C18 N11 N12 105.7(2) . . ?
N5 N6 B1 119.02(18) . . ?
C9 N6 N5 109.4(2) . . ?
C9 N6 B1 131.3(2) . . ?
N6 N5 Fe01 118.78(14) . . ?
C7 N5 Fe01 135.12(19) . . ?
C7 N5 N6 105.9(2) . . ?
N3 N4 B1 120.48(18) . . ?
C6 N4 N3 108.7(2) . . ?
C6 N4 B1 130.8(2) . . ?
N11 N12 B2 119.41(18) . . ?
C20 N12 N11 109.7(2) . . ?
C20 N12 B2 130.9(2) . . ?
N10 N9 Fe02 118.20(14) . . ?
C15 N9 Fe02 135.79(18) . . ?
C15 N9 N10 105.9(2) . . ?
N4 N3 Fe01 117.70(14) . . ?
C4 N3 Fe01 135.87(19) . . ?
C4 N3 N4 106.2(2) . . ?
N8 C14 C13 107.3(2) . . ?
N8 C14 C22 122.9(3) . . ?
C13 C14 C22 129.7(3) . . ?
C14 C13 H13 126.5 . . ?
C14 C13 C12 107.1(2) . . ?
C12 C13 H13 126.5 . . ?
N7 C12 C13 109.6(2) . . ?
N7 C12 C21 122.0(3) . . ?
C13 C12 C21 128.3(3) . . ?
N3 C4 H4 124.4 . . ?
N3 C4 C5 111.1(3) . . ?
C5 C4 H4 124.4 . . ?
N4 C6 H6 125.4 . . ?
N4 C6 C5 109.1(3) . . ?
C5 C6 H6 125.4 . . ?
N10 C17 H17 125.4 . . ?
N10 C17 C16 109.2(2) . . ?
C16 C17 H17 125.4 . . ?
C4 C5 H5 127.6 . . ?
C6 C5 C4 104.8(3) . . ?
C6 C5 H5 127.6 . . ?
N2 C3 C2 106.8(2) . . ?
N2 C3 C11 123.3(2) . . ?
C2 C3 C11 129.9(2) . . ?
N9 C15 H15 124.5 . . ?
N9 C15 C16 111.0(3) . . ?
C16 C15 H15 124.5 . . ?
N1 C1 C2 109.5(2) . . ?
N1 C1 C10 122.5(2) . . ?
C2 C1 C10 128.0(2) . . ?
C3 C2 C1 107.4(2) . . ?
C3 C2 H2 126.3 . . ?
C1 C2 H2 126.3 . . ?
C17 C16 C15 104.7(3) . . ?
C17 C16 H16 127.7 . . ?
C15 C16 H16 127.7 . . ?
N11 C18 H18 124.5 . . ?
N11 C18 C19 110.9(3) . . ?
C19 C18 H18 124.5 . . ?
N5 C7 H7 124.5 . . ?
N5 C7 C8 110.9(3) . . ?
C8 C7 H7 124.5 . . ?
N12 C20 H20 125.8 . . ?
N12 C20 C19 108.3(3) . . ?
C19 C20 H20 125.8 . . ?
N6 C9 H9 125.5 . . ?
N6 C9 C8 109.0(3) . . ?
C8 C9 H9 125.5 . . ?
C18 C19 H19 127.3 . . ?
C20 C19 C18 105.4(2) . . ?
C20 C19 H19 127.3 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.6 . . ?
C9 C8 C7 104.8(2) . . ?
C9 C8 H8 127.6 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 107.4(2) . . ?
N2 B1 H1 113.2(13) . . ?
N6 B1 H1 106.0(13) . . ?
N4 B1 N2 109.9(2) . . ?
N4 B1 N6 108.8(2) . . ?
N4 B1 H1 111.3(13) . . ?
N10 B2 H2A 108.4(13) . . ?
N8 B2 N10 108.91(19) . . ?
N8 B2 N12 109.2(2) . . ?
N8 B2 H2A 111.1(14) . . ?
N12 B2 N10 108.0(2) . . ?
N12 B2 H2A 111.2(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -172.96(18) . . . . ?
Fe01 N1 C1 C10 7.1(4) . . . . ?
Fe01 N5 C7 C8 174.37(19) . . . . ?
Fe01 N3 C4 C5 173.5(2) . . . . ?
Fe02 N7 N8 C14 -179.23(16) . . . . ?
Fe02 N7 N8 B2 0.0(3) . . . . ?
Fe02 N7 C12 C13 178.4(2) . . . . ?
Fe02 N7 C12 C21 -2.0(4) . . . . ?
Fe02 N11 N12 C20 173.90(16) . . . . ?
Fe02 N11 N12 B2 -4.6(3) . . . . ?
Fe02 N11 C18 C19 -172.5(2) . . . . ?
Fe02 N9 C15 C16 176.5(2) . . . . ?
N7 N8 C14 C13 0.7(3) . . . . ?
N7 N8 C14 C22 -179.8(2) . . . . ?
N7 N8 B2 N10 -58.7(3) . . . . ?
N7 N8 B2 N12 59.1(3) . . . . ?
N2 N1 C1 C2 0.6(3) . . . . ?
N2 N1 C1 C10 -179.4(2) . . . . ?
N2 C3 C2 C1 -0.2(3) . . . . ?
N10 N9 C15 C16 -0.5(3) . . . . ?
N10 C17 C16 C15 0.2(3) . . . . ?
N8 N7 C12 C13 -0.3(3) . . . . ?
N8 N7 C12 C21 179.3(3) . . . . ?
N8 C14 C13 C12 -0.9(3) . . . . ?
N1 N2 C3 C2 0.5(3) . . . . ?
N1 N2 C3 C11 -178.1(2) . . . . ?
N1 N2 B1 N6 62.4(3) . . . . ?
N1 N2 B1 N4 -55.9(3) . . . . ?
N1 C1 C2 C3 -0.3(3) . . . . ?
N11 N12 C20 C19 0.5(3) . . . . ?
N11 N12 B2 N10 61.3(3) . . . . ?
N11 N12 B2 N8 -56.9(3) . . . . ?
N11 C18 C19 C20 -0.6(3) . . . . ?
N6 N5 C7 C8 -0.3(3) . . . . ?
N6 C9 C8 C7 0.3(3) . . . . ?
N5 N6 C9 C8 -0.5(3) . . . . ?
N5 N6 B1 N2 -60.9(3) . . . . ?
N5 N6 B1 N4 58.0(3) . . . . ?
N5 C7 C8 C9 0.0(3) . . . . ?
N4 N3 C4 C5 -0.4(3) . . . . ?
N4 C6 C5 C4 0.5(4) . . . . ?
N12 N11 C18 C19 0.9(3) . . . . ?
N12 C20 C19 C18 0.0(3) . . . . ?
N9 N10 C17 C16 -0.5(3) . . . . ?
N9 N10 B2 N8 57.2(3) . . . . ?
N9 N10 B2 N12 -61.3(3) . . . . ?
N9 C15 C16 C17 0.2(4) . . . . ?
N3 N4 C6 C5 -0.8(3) . . . . ?
N3 N4 B1 N2 55.5(3) . . . . ?
N3 N4 B1 N6 -61.8(3) . . . . ?
N3 C4 C5 C6 0.0(4) . . . . ?
C14 N8 B2 N10 120.3(3) . . . . ?
C14 N8 B2 N12 -121.9(3) . . . . ?
C14 C13 C12 N7 0.8(3) . . . . ?
C14 C13 C12 C21 -178.9(3) . . . . ?
C12 N7 N8 C14 -0.3(3) . . . . ?
C12 N7 N8 B2 179.0(2) . . . . ?
C6 N4 N3 Fe01 -174.54(17) . . . . ?
C6 N4 N3 C4 0.7(3) . . . . ?
C6 N4 B1 N2 -124.4(3) . . . . ?
C6 N4 B1 N6 118.2(3) . . . . ?
C17 N10 N9 Fe02 -176.99(17) . . . . ?
C17 N10 N9 C15 0.6(3) . . . . ?
C17 N10 B2 N8 -121.5(3) . . . . ?
C17 N10 B2 N12 120.0(3) . . . . ?
C3 N2 N1 Fe01 174.28(14) . . . . ?
C3 N2 N1 C1 -0.7(2) . . . . ?
C3 N2 B1 N6 -114.5(2) . . . . ?
C3 N2 B1 N4 127.2(2) . . . . ?
C18 N11 N12 C20 -0.9(3) . . . . ?
C18 N11 N12 B2 -179.4(2) . . . . ?
C20 N12 B2 N10 -116.8(3) . . . . ?
C20 N12 B2 N8 124.9(3) . . . . ?
C9 N6 N5 Fe01 -175.21(16) . . . . ?
C9 N6 N5 C7 0.5(3) . . . . ?
C9 N6 B1 N2 112.9(3) . . . . ?
C9 N6 B1 N4 -128.1(3) . . . . ?
C22 C14 C13 C12 179.6(3) . . . . ?
C10 C1 C2 C3 179.7(3) . . . . ?
C11 C3 C2 C1 178.3(3) . . . . ?
B1 N2 N1 Fe01 -3.2(3) . . . . ?
B1 N2 N1 C1 -178.2(2) . . . . ?
B1 N2 C3 C2 177.7(2) . . . . ?
B1 N2 C3 C11 -1.0(4) . . . . ?
B1 N6 N5 Fe01 -0.1(3) . . . . ?
B1 N6 N5 C7 175.6(2) . . . . ?
B1 N6 C9 C8 -174.8(2) . . . . ?
B1 N4 N3 Fe01 5.5(3) . . . . ?
B1 N4 N3 C4 -179.2(2) . . . . ?
B1 N4 C6 C5 179.2(3) . . . . ?
B2 N10 N9 Fe02 4.0(3) . . . . ?
B2 N10 N9 C15 -178.4(2) . . . . ?
B2 N10 C17 C16 178.4(3) . . . . ?
B2 N8 C14 C13 -178.4(2) . . . . ?
B2 N8 C14 C22 1.2(4) . . . . ?
B2 N12 C20 C19 178.8(3) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_360K
_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_pr210_330kdown
_database_code_depnum_ccdc_archive 'CCDC 2261114'
loop_
_audit_author_name
_audit_author_address
'Patrick Rosa'
;ICMCB, CNRS, Universite de Bordeaux
France
;
_audit_update_record             
;
2023-05-06 deposited with the CCDC.	2023-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
margaux.penicaud@icmcb.cnrs.fr
edoardo.martinez@unifi.it
giulia.serrano@unifi.it
brunetto.cortigiani@unifi.it
''
''
''
mathieu.gonidec@icmcb.cnrs.fr
patrick.rosa@icmcb.cnrs.fr
matteo.mannini@unifi.it
lpoggini@iccom.cnr.it
_chemical_name_common            ?
_chemical_name_systematic        
'Iron(II) bis (bis(pyrazol-1-yl)(3,5-dimethylpyrazol-1-yl)borohydride)'
_chemical_formula_moiety         '2(C11 H14 B Fe0.5 N6)'
_chemical_formula_sum            'C22 H28 B2 Fe N12'
_chemical_formula_weight         538.03
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9257(7)
_cell_length_b                   10.8110(8)
_cell_length_c                   12.2594(9)
_cell_angle_alpha                93.045(5)
_cell_angle_beta                 94.963(5)
_cell_angle_gamma                95.384(5)
_cell_volume                     1302.31(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5107
_cell_measurement_temperature    330(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.41
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.791
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 
'Crystals were obtained by slow diffusion of a MeOH solution of the ligand in a MeOH solution of FeCl₂.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9959
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.400
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.533
_diffrn_ambient_temperature      330(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_special_details          
;
The data collection nominally covered a full sphere of reciprocal space by a combination of 3 sets of ω scans each set at different φ and/or 2θ angles and each scan (120.00 s exposure) covering 2.000\ degrees in ω.
 The crystal to detector distance was 2.6 cm.
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4096
_reflns_number_total             5887
_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       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.010
_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)+(0.0700P)²+0.0557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1255
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C6(H6), C17(H17), C5(H5), C15(H15), C2(H2), C16(H16),
 C18(H18), C7(H7), C20(H20), C9(H9), C19(H19), C8(H8)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe01 Fe 0.500000 0.500000 0.500000 0.04953(14) Uani 1 2 d S . P . .
Fe02 Fe 1.000000 1.000000 1.000000 0.05109(14) Uani 1 2 d S . P . .
N7 N 0.80539(19) 1.00741(18) 0.92500(16) 0.0627(5) Uani 1 1 d . . . . .
N2 N 0.78239(18) 0.55316(17) 0.43710(15) 0.0578(4) Uani 1 1 d . . . . .
N10 N 0.86234(19) 0.74540(17) 0.96509(16) 0.0602(5) Uani 1 1 d . . . . .
N8 N 0.70711(18) 0.91320(18) 0.94191(16) 0.0607(5) Uani 1 1 d . . . . .
N1 N 0.69668(18) 0.58832(17) 0.51350(15) 0.0581(4) Uani 1 1 d . . . . .
N11 N 0.9086(2) 0.95578(18) 1.13818(16) 0.0622(5) Uani 1 1 d . . . . .
N6 N 0.6069(2) 0.48994(18) 0.28200(15) 0.0613(5) Uani 1 1 d . . . . .
N5 N 0.49738(19) 0.51770(18) 0.33423(16) 0.0616(5) Uani 1 1 d . . . . .
N4 N 0.68258(19) 0.33064(18) 0.40861(16) 0.0615(5) Uani 1 1 d . . . . .
N12 N 0.80055(19) 0.86677(17) 1.12895(16) 0.0605(5) Uani 1 1 d . . . . .
N9 N 0.97923(19) 0.81570(17) 0.94878(16) 0.0623(5) Uani 1 1 d . . . . .
N3 N 0.5864(2) 0.33740(18) 0.48123(15) 0.0621(5) Uani 1 1 d . . . . .
C14 C 0.5881(2) 0.9318(3) 0.8854(2) 0.0700(6) Uani 1 1 d . . . . .
C13 C 0.6106(3) 1.0385(3) 0.8319(2) 0.0836(8) Uani 1 1 d . . . . .
H13 H 0.547225 1.074008 0.786140 0.100 Uiso 1 1 calc R U . . .
C12 C 0.7450(3) 1.0841(3) 0.8585(2) 0.0727(7) Uani 1 1 d . . . . .
C4 C 0.5673(3) 0.2246(2) 0.5193(2) 0.0786(7) Uani 1 1 d . . . . .
H4 H 0.507157 0.202807 0.570788 0.094 Uiso 1 1 calc R U . . .
C6 C 0.7194(3) 0.2139(2) 0.4017(2) 0.0778(7) Uani 1 1 d . . . . .
H6 H 0.782136 0.185274 0.356790 0.093 Uiso 1 1 calc R U . . .
C17 C 0.8712(3) 0.6275(2) 0.9309(2) 0.0766(7) Uani 1 1 d . . . . .
H17 H 0.804181 0.561916 0.933832 0.092 Uiso 1 1 calc R U . . .
C5 C 0.6488(3) 0.1446(3) 0.4720(3) 0.0914(9) Uani 1 1 d . . . . .
H5 H 0.654581 0.061233 0.485068 0.110 Uiso 1 1 calc R U . . .
C3 C 0.9009(2) 0.6271(2) 0.4509(2) 0.0624(6) Uani 1 1 d . . . . .
C15 C 1.0575(3) 0.7383(3) 0.9032(2) 0.0777(7) Uani 1 1 d . . . . .
H15 H 1.143705 0.761679 0.882442 0.093 Uiso 1 1 calc R U . . .
C1 C 0.7656(3) 0.6833(2) 0.57558(19) 0.0636(6) Uani 1 1 d . . . . .
C2 C 0.8929(3) 0.7091(2) 0.5381(2) 0.0704(6) Uani 1 1 d . . . . .
H2 H 0.960095 0.770791 0.567031 0.084 Uiso 1 1 calc R U . . .
C16 C 0.9942(3) 0.6185(3) 0.8908(3) 0.0875(8) Uani 1 1 d . . . . .
H16 H 1.027729 0.547666 0.861695 0.105 Uiso 1 1 calc R U . . .
C18 C 0.9347(3) 0.9879(3) 1.2442(2) 0.0770(7) Uani 1 1 d . . . . .
H18 H 1.002810 1.048285 1.273876 0.092 Uiso 1 1 calc R U . . .
C7 C 0.4122(3) 0.5597(3) 0.2587(2) 0.0770(7) Uani 1 1 d . . . . .
H7 H 0.327644 0.584877 0.271618 0.092 Uiso 1 1 calc R U . . .
C20 C 0.7636(3) 0.8437(2) 1.2294(2) 0.0731(7) Uani 1 1 d . . . . .
H20 H 0.693305 0.786202 1.245155 0.088 Uiso 1 1 calc R U . . .
C9 C 0.5886(3) 0.5163(3) 0.1765(2) 0.0779(8) Uani 1 1 d . . . . .
H9 H 0.649661 0.505834 0.124153 0.093 Uiso 1 1 calc R U . . .
C19 C 0.8471(3) 0.9195(3) 1.3044(2) 0.0867(8) Uani 1 1 d . . . . .
H19 H 0.845164 0.923986 1.380193 0.104 Uiso 1 1 calc R U . . .
C21 C 0.8175(3) 1.1987(3) 0.8222(3) 0.1035(11) Uani 1 1 d . . . . .
H21A H 0.782149 1.270344 0.854366 0.155 Uiso 1 1 calc R U . . .
H21B H 0.804697 1.199040 0.743735 0.155 Uiso 1 1 calc R U . . .
H21C H 0.912768 1.200845 0.845082 0.155 Uiso 1 1 calc R U . . .
C8 C 0.4651(3) 0.5613(3) 0.1589(2) 0.0890(9) Uani 1 1 d . . . . .
H8 H 0.425421 0.587276 0.093635 0.107 Uiso 1 1 calc R U . . .
C22 C 0.4612(3) 0.8456(3) 0.8867(3) 0.0989(10) Uani 1 1 d . . . . .
H22A H 0.474061 0.766049 0.852697 0.148 Uiso 1 1 calc R U . . .
H22B H 0.387033 0.879674 0.847159 0.148 Uiso 1 1 calc R U . . .
H22C H 0.441281 0.835779 0.961190 0.148 Uiso 1 1 calc R U . . .
C10 C 0.7093(3) 0.7480(3) 0.6692(2) 0.0841(8) Uani 1 1 d . . . . .
H10A H 0.689282 0.829629 0.649750 0.126 Uiso 1 1 calc R U . . .
H10B H 0.774814 0.755096 0.732177 0.126 Uiso 1 1 calc R U . . .
H10C H 0.627565 0.701120 0.686119 0.126 Uiso 1 1 calc R U . . .
C11 C 1.0131(3) 0.6141(3) 0.3778(2) 0.0798(7) Uani 1 1 d . . . . .
H11A H 1.035097 0.529463 0.374854 0.120 Uiso 1 1 calc R U . . .
H11B H 1.091899 0.668125 0.406536 0.120 Uiso 1 1 calc R U . . .
H11C H 0.984071 0.636366 0.305371 0.120 Uiso 1 1 calc R U . . .
B1 B 0.7308(3) 0.4471(3) 0.3510(2) 0.0618(6) Uani 1 1 d . . . . .
B2 B 0.7461(3) 0.8084(3) 1.0145(2) 0.0619(6) Uani 1 1 d . . . . .
H1 H 0.805(2) 0.429(2) 0.2940(19) 0.062(6) Uiso 1 1 d . . . . .
H2A H 0.658(2) 0.739(2) 1.019(2) 0.069(7) Uiso 1 1 d . . . . .


_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 2.0803(18) . ?
Fe01 N1 2.0803(18) 2_666 ?
Fe01 N5 2.0496(19) 2_666 ?
Fe01 N5 2.0495(19) . ?
Fe01 N3 2.038(2) 2_666 ?
Fe01 N3 2.038(2) . ?
Fe02 N7 2.0767(19) . ?
Fe02 N7 2.0767(19) 2_777 ?
Fe02 N11 2.0475(19) 2_777 ?
Fe02 N11 2.0474(19) . ?
Fe02 N9 2.043(2) 2_777 ?
Fe02 N9 2.043(2) . ?
N7 N8 1.379(2) . ?
N7 C12 1.338(3) . ?
N2 N1 1.381(2) . ?
N2 C3 1.352(3) . ?
N2 B1 1.536(3) . ?
N10 N9 1.362(2) . ?
N10 C17 1.333(3) . ?
N10 B2 1.545(3) . ?
N8 C14 1.355(3) . ?
N8 B2 1.534(3) . ?
N1 C1 1.341(3) . ?
N11 N12 1.365(3) . ?
N11 C18 1.324(3) . ?
N6 N5 1.357(3) . ?
N6 C9 1.340(3) . ?
N6 B1 1.553(3) . ?
N5 C7 1.327(3) . ?
N4 N3 1.365(3) . ?
N4 C6 1.347(3) . ?
N4 B1 1.534(3) . ?
N12 C20 1.345(3) . ?
N12 B2 1.540(4) . ?
N9 C15 1.328(3) . ?
N3 C4 1.332(3) . ?
C14 C13 1.366(4) . ?
C14 C22 1.496(4) . ?
C13 H13 0.9300 . ?
C13 C12 1.383(4) . ?
C12 C21 1.483(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.378(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.367(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.365(4) . ?
C5 H5 0.9300 . ?
C3 C2 1.365(4) . ?
C3 C11 1.500(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(4) . ?
C1 C2 1.391(3) . ?
C1 C10 1.490(4) . ?
C2 H2 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.377(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.372(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.365(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.365(4) . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
B1 H1 1.08(2) . ?
B2 H2A 1.10(2) . ?

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 180.0 2_666 . ?
N5 Fe01 N1 92.79(7) . 2_666 ?
N5 Fe01 N1 87.21(7) 2_666 2_666 ?
N5 Fe01 N1 87.21(7) . . ?
N5 Fe01 N1 92.79(7) 2_666 . ?
N5 Fe01 N5 180.0 . 2_666 ?
N3 Fe01 N1 86.54(8) . . ?
N3 Fe01 N1 86.54(8) 2_666 2_666 ?
N3 Fe01 N1 93.46(8) . 2_666 ?
N3 Fe01 N1 93.46(8) 2_666 . ?
N3 Fe01 N5 89.29(8) . . ?
N3 Fe01 N5 90.71(8) . 2_666 ?
N3 Fe01 N5 89.29(8) 2_666 2_666 ?
N3 Fe01 N5 90.71(8) 2_666 . ?
N3 Fe01 N3 180.0 2_666 . ?
N7 Fe02 N7 180.0 2_777 . ?
N11 Fe02 N7 86.53(8) . . ?
N11 Fe02 N7 93.47(8) 2_777 . ?
N11 Fe02 N7 86.53(8) 2_777 2_777 ?
N11 Fe02 N7 93.47(8) . 2_777 ?
N11 Fe02 N11 180.00(5) . 2_777 ?
N9 Fe02 N7 93.25(8) . 2_777 ?
N9 Fe02 N7 86.75(8) . . ?
N9 Fe02 N7 86.75(8) 2_777 2_777 ?
N9 Fe02 N7 93.25(8) 2_777 . ?
N9 Fe02 N11 89.44(8) 2_777 2_777 ?
N9 Fe02 N11 90.56(7) . 2_777 ?
N9 Fe02 N11 89.44(7) . . ?
N9 Fe02 N11 90.56(7) 2_777 . ?
N9 Fe02 N9 180.00(10) . 2_777 ?
N8 N7 Fe02 117.91(13) . . ?
C12 N7 Fe02 135.68(17) . . ?
C12 N7 N8 106.40(19) . . ?
N1 N2 B1 118.75(17) . . ?
C3 N2 N1 110.15(18) . . ?
C3 N2 B1 131.02(19) . . ?
N9 N10 B2 119.37(18) . . ?
C17 N10 N9 109.4(2) . . ?
C17 N10 B2 131.2(2) . . ?
N7 N8 B2 118.89(18) . . ?
C14 N8 N7 109.77(19) . . ?
C14 N8 B2 131.3(2) . . ?
N2 N1 Fe01 117.65(13) . . ?
C1 N1 Fe01 136.02(16) . . ?
C1 N1 N2 106.09(18) . . ?
N12 N11 Fe02 118.73(14) . . ?
C18 N11 Fe02 134.70(19) . . ?
C18 N11 N12 106.4(2) . . ?
N5 N6 B1 118.40(18) . . ?
C9 N6 N5 109.7(2) . . ?
C9 N6 B1 131.7(2) . . ?
N6 N5 Fe01 119.25(14) . . ?
C7 N5 Fe01 134.78(18) . . ?
C7 N5 N6 105.8(2) . . ?
N3 N4 B1 119.66(18) . . ?
C6 N4 N3 109.3(2) . . ?
C6 N4 B1 131.1(2) . . ?
N11 N12 B2 119.10(18) . . ?
C20 N12 N11 109.3(2) . . ?
C20 N12 B2 131.5(2) . . ?
N10 N9 Fe02 118.62(14) . . ?
C15 N9 Fe02 135.42(18) . . ?
C15 N9 N10 105.9(2) . . ?
N4 N3 Fe01 118.25(14) . . ?
C4 N3 Fe01 135.37(18) . . ?
C4 N3 N4 106.2(2) . . ?
N8 C14 C13 107.0(2) . . ?
N8 C14 C22 122.9(3) . . ?
C13 C14 C22 130.1(3) . . ?
C14 C13 H13 126.3 . . ?
C14 C13 C12 107.4(2) . . ?
C12 C13 H13 126.3 . . ?
N7 C12 C13 109.4(2) . . ?
N7 C12 C21 122.7(2) . . ?
C13 C12 C21 127.8(2) . . ?
N3 C4 H4 124.6 . . ?
N3 C4 C5 110.7(3) . . ?
C5 C4 H4 124.6 . . ?
N4 C6 H6 125.8 . . ?
N4 C6 C5 108.4(2) . . ?
C5 C6 H6 125.8 . . ?
N10 C17 H17 125.4 . . ?
N10 C17 C16 109.1(2) . . ?
C16 C17 H17 125.4 . . ?
C4 C5 H5 127.3 . . ?
C6 C5 C4 105.3(2) . . ?
C6 C5 H5 127.3 . . ?
N2 C3 C2 107.1(2) . . ?
N2 C3 C11 122.6(2) . . ?
C2 C3 C11 130.3(2) . . ?
N9 C15 H15 124.4 . . ?
N9 C15 C16 111.1(2) . . ?
C16 C15 H15 124.4 . . ?
N1 C1 C2 109.4(2) . . ?
N1 C1 C10 123.3(2) . . ?
C2 C1 C10 127.3(2) . . ?
C3 C2 C1 107.2(2) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C17 C16 C15 104.4(2) . . ?
C17 C16 H16 127.8 . . ?
C15 C16 H16 127.8 . . ?
N11 C18 H18 124.7 . . ?
N11 C18 C19 110.6(3) . . ?
C19 C18 H18 124.7 . . ?
N5 C7 H7 124.4 . . ?
N5 C7 C8 111.2(3) . . ?
C8 C7 H7 124.4 . . ?
N12 C20 H20 125.9 . . ?
N12 C20 C19 108.1(2) . . ?
C19 C20 H20 125.9 . . ?
N6 C9 H9 125.8 . . ?
N6 C9 C8 108.4(2) . . ?
C8 C9 H9 125.8 . . ?
C18 C19 H19 127.2 . . ?
C20 C19 C18 105.6(2) . . ?
C20 C19 H19 127.2 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8 127.5 . . ?
C9 C8 C7 104.9(2) . . ?
C9 C8 H8 127.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 B1 N6 107.2(2) . . ?
N2 B1 H1 112.6(12) . . ?
N6 B1 H1 106.4(12) . . ?
N4 B1 N2 109.61(19) . . ?
N4 B1 N6 108.35(19) . . ?
N4 B1 H1 112.3(12) . . ?
N10 B2 H2A 109.9(13) . . ?
N8 B2 N10 108.56(18) . . ?
N8 B2 N12 108.3(2) . . ?
N8 B2 H2A 110.7(13) . . ?
N12 B2 N10 107.9(2) . . ?
N12 B2 H2A 111.4(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N1 C1 C2 -173.26(17) . . . . ?
Fe01 N1 C1 C10 6.6(4) . . . . ?
Fe01 N5 C7 C8 174.55(19) . . . . ?
Fe01 N3 C4 C5 175.0(2) . . . . ?
Fe02 N7 N8 C14 -178.78(16) . . . . ?
Fe02 N7 N8 B2 -0.1(3) . . . . ?
Fe02 N7 C12 C13 178.20(19) . . . . ?
Fe02 N7 C12 C21 -1.7(4) . . . . ?
Fe02 N11 N12 C20 174.45(15) . . . . ?
Fe02 N11 N12 B2 -3.5(3) . . . . ?
Fe02 N11 C18 C19 -173.47(19) . . . . ?
Fe02 N9 C15 C16 176.5(2) . . . . ?
N7 N8 C14 C13 0.1(3) . . . . ?
N7 N8 C14 C22 -180.0(2) . . . . ?
N7 N8 B2 N10 -58.1(3) . . . . ?
N7 N8 B2 N12 58.8(3) . . . . ?
N2 N1 C1 C2 0.7(3) . . . . ?
N2 N1 C1 C10 -179.4(2) . . . . ?
N2 C3 C2 C1 -0.7(3) . . . . ?
N10 N9 C15 C16 -0.7(3) . . . . ?
N10 C17 C16 C15 -0.1(3) . . . . ?
N8 N7 C12 C13 -0.9(3) . . . . ?
N8 N7 C12 C21 179.1(3) . . . . ?
N8 C14 C13 C12 -0.6(3) . . . . ?
N1 N2 C3 C2 1.2(3) . . . . ?
N1 N2 C3 C11 -178.2(2) . . . . ?
N1 N2 B1 N6 61.8(2) . . . . ?
N1 N2 B1 N4 -55.6(3) . . . . ?
N1 C1 C2 C3 -0.1(3) . . . . ?
N11 N12 C20 C19 0.8(3) . . . . ?
N11 N12 B2 N10 60.2(3) . . . . ?
N11 N12 B2 N8 -57.2(3) . . . . ?
N11 C18 C19 C20 -0.7(3) . . . . ?
N6 N5 C7 C8 -0.8(3) . . . . ?
N6 C9 C8 C7 -0.1(3) . . . . ?
N5 N6 C9 C8 -0.4(3) . . . . ?
N5 N6 B1 N2 -60.0(3) . . . . ?
N5 N6 B1 N4 58.2(3) . . . . ?
N5 C7 C8 C9 0.6(3) . . . . ?
N4 N3 C4 C5 -0.4(3) . . . . ?
N4 C6 C5 C4 0.9(3) . . . . ?
N12 N11 C18 C19 1.2(3) . . . . ?
N12 C20 C19 C18 -0.1(3) . . . . ?
N9 N10 C17 C16 -0.3(3) . . . . ?
N9 N10 B2 N8 56.6(3) . . . . ?
N9 N10 B2 N12 -60.6(3) . . . . ?
N9 C15 C16 C17 0.5(3) . . . . ?
N3 N4 C6 C5 -1.2(3) . . . . ?
N3 N4 B1 N2 55.5(3) . . . . ?
N3 N4 B1 N6 -61.2(3) . . . . ?
N3 C4 C5 C6 -0.3(4) . . . . ?
C14 N8 B2 N10 120.2(3) . . . . ?
C14 N8 B2 N12 -122.9(3) . . . . ?
C14 C13 C12 N7 1.0(3) . . . . ?
C14 C13 C12 C21 -179.1(3) . . . . ?
C12 N7 N8 C14 0.5(3) . . . . ?
C12 N7 N8 B2 179.2(2) . . . . ?
C6 N4 N3 Fe01 -175.31(17) . . . . ?
C6 N4 N3 C4 1.0(3) . . . . ?
C6 N4 B1 N2 -124.2(3) . . . . ?
C6 N4 B1 N6 119.1(3) . . . . ?
C17 N10 N9 Fe02 -177.16(17) . . . . ?
C17 N10 N9 C15 0.6(3) . . . . ?
C17 N10 B2 N8 -122.0(3) . . . . ?
C17 N10 B2 N12 120.8(3) . . . . ?
C3 N2 N1 Fe01 174.12(14) . . . . ?
C3 N2 N1 C1 -1.2(2) . . . . ?
C3 N2 B1 N6 -114.8(2) . . . . ?
C3 N2 B1 N4 127.8(2) . . . . ?
C18 N11 N12 C20 -1.2(3) . . . . ?
C18 N11 N12 B2 -179.2(2) . . . . ?
C20 N12 B2 N10 -117.3(3) . . . . ?
C20 N12 B2 N8 125.3(2) . . . . ?
C9 N6 N5 Fe01 -175.49(16) . . . . ?
C9 N6 N5 C7 0.7(3) . . . . ?
C9 N6 B1 N2 113.4(3) . . . . ?
C9 N6 B1 N4 -128.4(3) . . . . ?
C22 C14 C13 C12 179.4(3) . . . . ?
C10 C1 C2 C3 -179.9(3) . . . . ?
C11 C3 C2 C1 178.6(2) . . . . ?
B1 N2 N1 Fe01 -3.2(2) . . . . ?
B1 N2 N1 C1 -178.5(2) . . . . ?
B1 N2 C3 C2 178.0(2) . . . . ?
B1 N2 C3 C11 -1.3(4) . . . . ?
B1 N6 N5 Fe01 -0.7(3) . . . . ?
B1 N6 N5 C7 175.5(2) . . . . ?
B1 N6 C9 C8 -174.3(2) . . . . ?
B1 N4 N3 Fe01 4.9(3) . . . . ?
B1 N4 N3 C4 -178.7(2) . . . . ?
B1 N4 C6 C5 178.5(3) . . . . ?
B2 N10 N9 Fe02 4.0(3) . . . . ?
B2 N10 N9 C15 -178.2(2) . . . . ?
B2 N10 C17 C16 178.4(2) . . . . ?
B2 N8 C14 C13 -178.4(2) . . . . ?
B2 N8 C14 C22 1.6(4) . . . . ?
B2 N12 C20 C19 178.4(2) . . . . ?


_olex2_date_sample_data_collection 2017-09-01
_olex2_exptl_crystal_mounting_method 
'The crystal was glued with nail varnish to a glass fiber.'
_olex2_submission_original_sample_id PR210_330Kdown
_olex2_submission_special_instructions 'No special instructions were received'
