# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_fmm_tm52017k
_database_code_depnum_ccdc_archive 'CCDC 1860121'
loop_
_audit_author_name
_audit_author_address
'Francesco Monzittu'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2018-08-03 deposited with the CCDC.	2019-03-19 downloaded from the CCDC.
;
_audit_creation_date             2017-11-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9.01 H21 F3 Mn N3, 4(H2 O)'
_chemical_formula_sum            'C9 H29 F3 Mn N3 O4'
_chemical_formula_weight         355.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         C9H25MnF3N3O2
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.9041(2)
_cell_length_b                   13.2669(3)
_cell_length_c                   26.9700(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3185.96(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9349
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.0460
_cell_measurement_theta_min      3.1240
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.949
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32812
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.857
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00  15.00   1.00   15.00    --  -19.30 -37.00 -30.00  124
  2  ω    -55.00  70.00   1.00   15.00    --  -19.30  57.00  30.00  125
  3  ω    -58.00  70.00   1.00   15.00    --  -19.30  72.00-150.00  128
  4  ω    -58.00 -33.00   1.00   15.00    --  -19.30  72.00  90.00   25
  5  ω   -109.00  19.00   1.00   15.00    --  -19.30 -72.00 150.00  128
;
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236169000
_diffrn_orient_matrix_UB_12      -0.0453201000
_diffrn_orient_matrix_UB_13      0.0115545000
_diffrn_orient_matrix_UB_21      0.0716796000
_diffrn_orient_matrix_UB_22      0.0215369000
_diffrn_orient_matrix_UB_23      0.0044619000
_diffrn_orient_matrix_UB_31      -0.0254950000
_diffrn_orient_matrix_UB_32      0.0184547000
_diffrn_orient_matrix_UB_33      0.0232005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3023
_reflns_number_total             3124
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     273
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0663
_refine_ls_restrained_S_all      1.353
_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)+(0.0236P)²+7.1874P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1170
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(3)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(3)
5.a Free rotating group:
 O4(H4C,H4D), O2(H2C,H2D), O3(H3C,H3D), O1(H1C,H1D)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C4(H4A,H4B), C1(H1A,H1B), C3(H3A,H3B), C6(H6A,H6B),
 C6A(H6AA,H6AB), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C4A(H4AA,H4AB), C3A(H3AA,H3AB),
  C5A(H5AA,H5AB)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.73363(5) 0.06938(4) 0.35592(2) 0.01197(15) Uani 1 1 d . U . . .
F1 F 0.5565(2) 0.10641(15) 0.31302(7) 0.0187(5) Uani 1 1 d . U . . .
F2 F 0.6920(2) 0.16523(14) 0.40393(7) 0.0201(5) Uani 1 1 d . U . . .
F3 F 0.8682(2) 0.15072(15) 0.32248(7) 0.0198(5) Uani 1 1 d . U . . .
O4 O 0.6010(3) 0.22166(19) 0.23116(9) 0.0189(6) Uani 1 1 d . U . . .
H4C H 0.601663 0.187637 0.257820 0.028 Uiso 1 1 d G . . . .
H4D H 0.529141 0.201877 0.212800 0.028 Uiso 1 1 d G . . . .
N1 N 0.7880(3) -0.0504(2) 0.30949(10) 0.0140(6) Uani 1 1 d . U . . .
N2 N 0.9230(4) 0.0008(2) 0.40086(11) 0.0193(7) Uani 1 1 d . U . . .
N3 N 0.6106(3) -0.0407(2) 0.39412(11) 0.0171(6) Uani 1 1 d . U . . .
C7 C 0.7915(4) -0.0190(3) 0.25670(13) 0.0208(8) Uani 1 1 d . U . . .
H7A H 0.697534 0.015561 0.248358 0.031 Uiso 1 1 calc GR . . . .
H7B H 0.802976 -0.078610 0.235584 0.031 Uiso 1 1 calc GR . . . .
H7C H 0.876262 0.026810 0.251278 0.031 Uiso 1 1 calc GR . . . .
C8 C 1.0212(4) 0.0781(3) 0.42231(15) 0.0270(9) Uani 1 1 d . U . . .
H8A H 1.064256 0.119251 0.395680 0.040 Uiso 1 1 calc GR . . . .
H8B H 1.102291 0.045593 0.440961 0.040 Uiso 1 1 calc GR . . . .
H8C H 0.962708 0.121215 0.444629 0.040 Uiso 1 1 calc GR . . . .
C9 C 0.4613(4) -0.0024(3) 0.40998(15) 0.0227(8) Uani 1 1 d . U . . .
H9A H 0.474843 0.054956 0.432412 0.034 Uiso 1 1 calc GR . . . .
H9B H 0.406604 -0.056132 0.427195 0.034 Uiso 1 1 calc GR . . . .
H9C H 0.404111 0.019051 0.380801 0.034 Uiso 1 1 calc GR . . . .
O2 O 0.5520(3) 0.2098(2) 0.48970(10) 0.0281(7) Uani 1 1 d . U . . .
H2C H 0.604972 0.197253 0.464262 0.042 Uiso 1 1 d G . . . .
H2D H 0.615554 0.220633 0.512611 0.042 Uiso 1 1 d G . . . .
O3 O 0.3184(3) 0.2163(2) 0.34366(9) 0.0264(6) Uani 1 1 d . U . . .
H3C H 0.256602 0.222934 0.319795 0.040 Uiso 1 1 d G . . . .
H3D H 0.390384 0.178410 0.334650 0.040 Uiso 1 1 d G . . . .
O1 O 1.2197(3) -0.2333(3) 0.44297(10) 0.0378(8) Uani 1 1 d . U . . .
H1C H 1.137702 -0.247850 0.457401 0.057 Uiso 1 1 d G . . . .
H1D H 1.207029 -0.252684 0.413230 0.057 Uiso 1 1 d G . . . .
C5 C 0.6063(11) -0.1352(6) 0.3671(4) 0.0192(19) Uani 0.59(2) 1 d . U P A 1
H5A H 0.505226 -0.165788 0.369841 0.023 Uiso 0.59(2) 1 calc R . P A 1
H5B H 0.680257 -0.182881 0.381319 0.023 Uiso 0.59(2) 1 calc R . P A 1
C2 C 1.0188(8) -0.0462(7) 0.3585(3) 0.0190(18) Uani 0.618(17) 1 d . U P A 1
H2A H 1.067979 0.008166 0.339233 0.023 Uiso 0.618(17) 1 calc R . P A 1
H2B H 1.098305 -0.089397 0.372852 0.023 Uiso 0.618(17) 1 calc R . P A 1
C4 C 0.7013(7) -0.0526(7) 0.4438(3) 0.0155(17) Uani 0.597(16) 1 d . U P A 1
H4A H 0.691634 0.009781 0.463622 0.019 Uiso 0.597(16) 1 calc R . P A 1
H4B H 0.658545 -0.108894 0.463294 0.019 Uiso 0.597(16) 1 calc R . P A 1
C1 C 0.9212(9) -0.1079(7) 0.3247(3) 0.0191(18) Uani 0.618(17) 1 d . U P A 1
H1A H 0.979254 -0.127798 0.295011 0.023 Uiso 0.618(17) 1 calc R . P A 1
H1B H 0.889322 -0.170044 0.342099 0.023 Uiso 0.618(17) 1 calc R . P A 1
C3 C 0.8663(10) -0.0732(7) 0.4337(3) 0.0204(18) Uani 0.597(16) 1 d . U P A 1
H3A H 0.923273 -0.071584 0.465197 0.025 Uiso 0.597(16) 1 calc R . P A 1
H3B H 0.878076 -0.140991 0.418827 0.025 Uiso 0.597(16) 1 calc R . P A 1
C6 C 0.6434(12) -0.1149(8) 0.3129(3) 0.0174(19) Uani 0.59(2) 1 d . U P A 1
H6A H 0.558912 -0.078785 0.296906 0.021 Uiso 0.59(2) 1 calc R . P A 1
H6B H 0.658397 -0.179535 0.295185 0.021 Uiso 0.59(2) 1 calc R . P A 1
C6A C 0.702(2) -0.1406(10) 0.3208(5) 0.019(3) Uani 0.41(2) 1 d . U P A 2
H6AA H 0.764077 -0.187430 0.340699 0.022 Uiso 0.41(2) 1 calc R . P A 2
H6AB H 0.673663 -0.175090 0.289633 0.022 Uiso 0.41(2) 1 calc R . P A 2
C1A C 0.5641(17) -0.1131(11) 0.3490(5) 0.018(3) Uani 0.41(2) 1 d . U P A 2
H1AA H 0.515149 -0.174772 0.361964 0.021 Uiso 0.41(2) 1 calc R . P A 2
H1AB H 0.492119 -0.078130 0.326967 0.021 Uiso 0.41(2) 1 calc R . P A 2
C2A C 0.9853(13) -0.0842(10) 0.3764(5) 0.018(3) Uani 0.382(17) 1 d . U P A 2
H2AA H 0.935853 -0.146847 0.387771 0.021 Uiso 0.382(17) 1 calc R . P A 2
H2AB H 1.094220 -0.089262 0.383358 0.021 Uiso 0.382(17) 1 calc R . P A 2
C4A C 0.9585(14) -0.0684(12) 0.3212(4) 0.019(3) Uani 0.39(2) 1 d . U . A 2
H4AA H 0.993927 -0.128426 0.302754 0.023 Uiso 0.382(17) 1 calc R . P A 2
H4AB H 1.017478 -0.009601 0.309706 0.023 Uiso 0.382(17) 1 calc R . P A 2
C3A C 0.6922(11) -0.0974(9) 0.4306(4) 0.016(2) Uani 0.403(16) 1 d . U P A 2
H3AA H 0.725245 -0.162416 0.416273 0.019 Uiso 0.403(16) 1 calc R . P A 2
H3AB H 0.626521 -0.111825 0.459376 0.019 Uiso 0.403(16) 1 calc R . P A 2
C5A C 0.8265(14) -0.0376(11) 0.4472(5) 0.020(3) Uani 0.403(16) 1 d . U P A 2
H5AA H 0.890421 -0.080060 0.468747 0.024 Uiso 0.403(16) 1 calc R . P A 2
H5AB H 0.792543 0.021162 0.466814 0.024 Uiso 0.403(16) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 F1 2.017(2) . ?
Mn1 F2 1.852(2) . ?
Mn1 F3 1.848(2) . ?
Mn1 N1 2.080(3) . ?
Mn1 N2 2.267(3) . ?
Mn1 N3 2.096(3) . ?
O4 H4C 0.8490 . ?
O4 H4D 0.8504 . ?
N1 C7 1.484(4) . ?
N1 C1 1.469(7) . ?
N1 C6 1.549(8) . ?
N1 C6A 1.453(11) . ?
N1 C4A 1.569(12) . ?
N2 C8 1.467(5) . ?
N2 C2 1.557(8) . ?
N2 C3 1.415(8) . ?
N2 C2A 1.419(10) . ?
N2 C5A 1.599(12) . ?
N3 C9 1.485(5) . ?
N3 C5 1.451(8) . ?
N3 C4 1.572(7) . ?
N3 C1A 1.605(11) . ?
N3 C3A 1.437(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O2 H2C 0.8492 . ?
O2 H2D 0.8502 . ?
O3 H3C 0.8513 . ?
O3 H3D 0.8504 . ?
O1 H1C 0.8498 . ?
O1 H1D 0.8500 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.524(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.501(11) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.518(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C6A C1A 1.49(2) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A C4A 1.523(18) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C5A 1.503(17) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?

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
F1 Mn1 N1 91.29(10) . . ?
F1 Mn1 N2 170.42(10) . . ?
F1 Mn1 N3 92.46(10) . . ?
F2 Mn1 F1 94.43(9) . . ?
F2 Mn1 N1 172.65(10) . . ?
F2 Mn1 N2 92.91(10) . . ?
F2 Mn1 N3 91.71(10) . . ?
F3 Mn1 F1 94.88(9) . . ?
F3 Mn1 F2 94.02(9) . . ?
F3 Mn1 N1 90.08(10) . . ?
F3 Mn1 N2 90.74(11) . . ?
F3 Mn1 N3 170.31(11) . . ?
N1 Mn1 N2 80.92(11) . . ?
N1 Mn1 N3 83.43(11) . . ?
N3 Mn1 N2 81.17(11) . . ?
H4C O4 H4D 109.5 . . ?
C7 N1 Mn1 111.6(2) . . ?
C7 N1 C6 103.2(4) . . ?
C7 N1 C4A 102.4(5) . . ?
C1 N1 Mn1 114.6(3) . . ?
C1 N1 C7 113.4(4) . . ?
C1 N1 C6 111.6(7) . . ?
C6 N1 Mn1 101.2(4) . . ?
C6A N1 Mn1 112.3(5) . . ?
C6A N1 C7 116.3(6) . . ?
C6A N1 C4A 110.0(10) . . ?
C4A N1 Mn1 102.8(5) . . ?
C8 N2 Mn1 111.9(2) . . ?
C8 N2 C2 104.1(4) . . ?
C8 N2 C5A 103.6(5) . . ?
C2 N2 Mn1 100.1(3) . . ?
C3 N2 Mn1 110.3(4) . . ?
C3 N2 C8 116.8(4) . . ?
C3 N2 C2 112.2(6) . . ?
C2A N2 Mn1 111.2(5) . . ?
C2A N2 C8 120.4(6) . . ?
C2A N2 C5A 108.7(9) . . ?
C5A N2 Mn1 98.4(5) . . ?
C9 N3 Mn1 111.8(2) . . ?
C9 N3 C4 104.4(4) . . ?
C9 N3 C1A 101.1(6) . . ?
C5 N3 Mn1 111.7(4) . . ?
C5 N3 C9 114.6(4) . . ?
C5 N3 C4 110.7(7) . . ?
C4 N3 Mn1 102.7(3) . . ?
C1A N3 Mn1 100.3(5) . . ?
C3A N3 Mn1 115.9(4) . . ?
C3A N3 C9 115.7(5) . . ?
C3A N3 C1A 109.6(9) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H2C O2 H2D 104.5 . . ?
H3C O3 H3D 109.4 . . ?
H1C O1 H1D 104.4 . . ?
N3 C5 H5A 109.9 . . ?
N3 C5 H5B 109.9 . . ?
N3 C5 C6 108.9(8) . . ?
H5A C5 H5B 108.3 . . ?
C6 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
N2 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 N2 110.2(6) . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
N3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C3 C4 N3 111.3(6) . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
N1 C1 C2 110.7(6) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C3 C4 109.4(7) . . ?
N2 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N1 C6 H6A 109.8 . . ?
N1 C6 H6B 109.8 . . ?
C5 C6 N1 109.5(7) . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
N1 C6A H6AA 109.7 . . ?
N1 C6A H6AB 109.7 . . ?
N1 C6A C1A 109.9(12) . . ?
H6AA C6A H6AB 108.2 . . ?
C1A C6A H6AA 109.7 . . ?
C1A C6A H6AB 109.7 . . ?
N3 C1A H1AA 109.9 . . ?
N3 C1A H1AB 109.9 . . ?
C6A C1A N3 108.7(11) . . ?
C6A C1A H1AA 109.9 . . ?
C6A C1A H1AB 109.9 . . ?
H1AA C1A H1AB 108.3 . . ?
N2 C2A H2AA 110.4 . . ?
N2 C2A H2AB 110.4 . . ?
N2 C2A C4A 106.5(11) . . ?
H2AA C2A H2AB 108.6 . . ?
C4A C2A H2AA 110.4 . . ?
C4A C2A H2AB 110.4 . . ?
N1 C4A H4AA 109.3 . . ?
N1 C4A H4AB 109.3 . . ?
C2A C4A N1 111.7(10) . . ?
C2A C4A H4AA 109.3 . . ?
C2A C4A H4AB 109.3 . . ?
H4AA C4A H4AB 107.9 . . ?
N3 C3A H3AA 109.8 . . ?
N3 C3A H3AB 109.8 . . ?
N3 C3A C5A 109.2(9) . . ?
H3AA C3A H3AB 108.3 . . ?
C5A C3A H3AA 109.8 . . ?
C5A C3A H3AB 109.8 . . ?
N2 C5A H5AA 109.4 . . ?
N2 C5A H5AB 109.4 . . ?
C3A C5A N2 111.3(9) . . ?
C3A C5A H5AA 109.4 . . ?
C3A C5A H5AB 109.4 . . ?
H5AA C5A H5AB 108.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.777
####################################################################### 
# 
# 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_2017fmm-8148-32k
_database_code_depnum_ccdc_archive 'CCDC 1860123'
loop_
_audit_author_name
_audit_author_address
'Francesco Monzittu'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2018-08-03 deposited with the CCDC.	2019-03-19 downloaded from the CCDC.
;
_audit_creation_date             2017-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H20.75 Co F3 N3, 4(H2 O)'
_chemical_formula_sum            'C9 H28.75 Co F3 N3 O4'
_chemical_formula_weight         359.03
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.74923(7)
_cell_length_b                   13.14407(11)
_cell_length_c                   26.2569(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3019.55(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19978
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.4960
_cell_measurement_theta_min      3.1820
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.932
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear purple'
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1518
_exptl_crystal_recrystallization_method MiTegen
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30727
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.902
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00  70.00   0.50   10.00    --  -19.10  57.00  30.00  248
  2  ω   -108.00  16.00   0.50   10.00    --  -19.10 -57.00 -90.00  248
  3  ω   -108.00  14.00   0.50   10.00    --  -19.10 -38.00  30.00  244
  4  ω    -52.00  70.00   0.50   10.00    --  -19.10  38.00   0.00  244
  5  ω    -57.00 -30.00   0.50   10.00    --  -19.10  72.00 150.00   54
;
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254037000
_diffrn_orient_matrix_UB_12      0.0169204000
_diffrn_orient_matrix_UB_13      0.0242176000
_diffrn_orient_matrix_UB_21      0.0757053000
_diffrn_orient_matrix_UB_22      -0.0148367000
_diffrn_orient_matrix_UB_23      -0.0062054000
_diffrn_orient_matrix_UB_31      0.0141540000
_diffrn_orient_matrix_UB_32      0.0490276000
_diffrn_orient_matrix_UB_33      -0.0102332000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2971
_reflns_number_total             2973
_reflns_odcompleteness_completeness 97.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.380
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2973
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0586
_refine_ls_restrained_S_all      1.328
_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)+(0.0333P)²+12.0373P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1427
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C11A)=Sof(H11A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=1-FVAR(3)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(3)
4.a Free rotating group:
 O1(H1C,H1D), O2(H2C,H2D), O3(H3C,H3D), O4(H4C,H4D)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B), C1(H1A,H1B),
 C9A(H9AA,H9AB), C15A(H15A,H15B), C8A(H8AA,H8AB), C14A(H14A,H14B), C13A(H13A,
 H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C11A(H11A)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Co1 Co 0.22839(6) 0.05472(4) 0.35682(2) 0.01990(18) Uani 1 1 d . U . . .
N2 N 0.2695(4) -0.0590(3) 0.31051(14) 0.0257(8) Uani 1 1 d . U . . .
F2 F 0.1884(3) 0.16148(18) 0.40201(9) 0.0274(6) Uani 1 1 d . U . . .
F3 F 0.0637(3) 0.0968(2) 0.31655(10) 0.0309(6) Uani 1 1 d . U . . .
F1 F 0.3532(4) 0.1400(2) 0.31875(11) 0.0382(7) Uani 1 1 d . U . . .
N3 N 0.4037(4) 0.0087(3) 0.39701(13) 0.0252(8) Uani 1 1 d . U . . .
N1 N 0.1010(4) -0.0386(3) 0.39668(15) 0.0281(8) Uani 1 1 d . U . . .
C8 C 0.2759(6) -0.0290(4) 0.25615(17) 0.0343(11) Uani 1 1 d . U . A 1
H8A H 0.184255 0.007009 0.247274 0.051 Uiso 1 1 calc GR . . A 1
H8B H 0.284712 -0.088847 0.235373 0.051 Uiso 1 1 calc GR . . A 1
H8C H 0.362840 0.014090 0.250592 0.051 Uiso 1 1 calc GR . . A 1
C2 C 0.1288(12) -0.1254(6) 0.3163(3) 0.0318(18) Uani 0.76(2) 1 d . U P A 1
H2A H 0.042516 -0.094032 0.299287 0.038 Uiso 0.76(2) 1 calc R . P A 1
H2B H 0.146935 -0.191350 0.300841 0.038 Uiso 0.76(2) 1 calc R . P A 1
C5 C 0.3548(10) -0.0630(8) 0.4364(3) 0.030(2) Uani 0.75(2) 1 d . U P A 1
H5A H 0.415179 -0.053512 0.467004 0.036 Uiso 0.75(2) 1 calc R . P A 1
H5B H 0.368888 -0.132375 0.424641 0.036 Uiso 0.75(2) 1 calc R . P A 1
C7 C -0.0517(5) 0.0022(4) 0.4086(2) 0.0353(11) Uani 1 1 d . U . B 1
H7A H -0.041304 0.065681 0.426349 0.053 Uiso 1 1 calc GR . . B 1
H7B H -0.105955 -0.045357 0.429652 0.053 Uiso 1 1 calc GR . . B 1
H7C H -0.107426 0.012892 0.377554 0.053 Uiso 1 1 calc GR . . B 1
C6 C 0.1882(9) -0.0438(9) 0.4476(3) 0.034(2) Uani 0.75(2) 1 d . U P A 1
H6A H 0.176736 0.019801 0.465976 0.041 Uiso 0.75(2) 1 calc R . P A 1
H6B H 0.147474 -0.098178 0.468545 0.041 Uiso 0.75(2) 1 calc R . P A 1
C9 C 0.4953(6) 0.0941(4) 0.41736(18) 0.0352(11) Uani 1 1 d . U . C 1
H9A H 0.523568 0.138798 0.390000 0.053 Uiso 1 1 calc GR . . C 1
H9B H 0.585865 0.068048 0.433352 0.053 Uiso 1 1 calc GR . . C 1
H9C H 0.435923 0.131054 0.441931 0.053 Uiso 1 1 calc GR . . C 1
C4 C 0.5060(8) -0.0436(7) 0.3582(3) 0.0268(17) Uani 0.77(2) 1 d . U P A 1
H4A H 0.553060 0.006546 0.336109 0.032 Uiso 0.77(2) 1 calc R . P A 1
H4B H 0.586281 -0.081118 0.375418 0.032 Uiso 0.77(2) 1 calc R . P A 1
C3 C 0.4077(10) -0.1153(7) 0.3274(3) 0.0268(17) Uani 0.77(2) 1 d . U P A 1
H3A H 0.464137 -0.139760 0.298041 0.032 Uiso 0.77(2) 1 calc R . P A 1
H3B H 0.378377 -0.173367 0.347957 0.032 Uiso 0.77(2) 1 calc R . P A 1
C1 C 0.0946(9) -0.1382(5) 0.3716(5) 0.035(2) Uani 0.76(2) 1 d . U P A 1
H1A H -0.006280 -0.167641 0.375821 0.042 Uiso 0.76(2) 1 calc R . P A 1
H1B H 0.168620 -0.183794 0.386924 0.042 Uiso 0.76(2) 1 calc R . P A 1
O1 O 0.1039(4) 0.2092(3) 0.23168(13) 0.0354(8) Uani 1 1 d . U . . .
H1C H 0.149777 0.194758 0.259258 0.053 Uiso 1 1 d G . . . .
H1D H 0.028859 0.168778 0.227617 0.053 Uiso 1 1 d G . . . .
O2 O -0.1762(4) 0.2203(3) 0.34282(12) 0.0344(8) Uani 1 1 d . U . . .
H2C H -0.240961 0.211820 0.319001 0.052 Uiso 1 1 d G . . . .
H2D H -0.096952 0.184931 0.336642 0.052 Uiso 1 1 d G . . . .
O3 O 0.0558(4) 0.2156(3) 0.48753(12) 0.0353(8) Uani 1 1 d . U . . .
H3C H 0.123384 0.222129 0.510589 0.053 Uiso 1 1 d G . . . .
H3D H 0.098485 0.199327 0.459627 0.053 Uiso 1 1 d G . . . .
O4 O 0.7147(4) -0.2201(3) 0.44239(14) 0.0447(10) Uani 1 1 d . U . . .
H4C H 0.635708 -0.245592 0.456332 0.067 Uiso 1 1 d G . . . .
H4D H 0.715790 -0.245548 0.412642 0.067 Uiso 1 1 d G . . . .
C11A C 0.178(3) -0.097(2) 0.4338(10) 0.038(6) Uani 0.25(2) 1 d . U P A 2
H11A H 0.152748 -0.161251 0.446422 0.045 Uiso 0.25(2) 1 calc R . P A 2
C9A C 0.314(3) -0.0293(18) 0.4480(8) 0.022(4) Uani 0.25(2) 1 d . U P A 2
H9AA H 0.384007 -0.066838 0.469677 0.027 Uiso 0.25(2) 1 calc R . P A 2
H9AB H 0.277931 0.029385 0.466914 0.027 Uiso 0.25(2) 1 calc R . P A 2
C15A C 0.050(4) -0.117(2) 0.3500(11) 0.034(6) Uani 0.24(2) 1 d . U P A 2
H15A H -0.002796 -0.176149 0.363900 0.041 Uiso 0.24(2) 1 calc R . P A 2
H15B H -0.018917 -0.083051 0.326541 0.041 Uiso 0.24(2) 1 calc R . P A 2
C8A C 0.193(4) -0.150(2) 0.3229(9) 0.030(5) Uani 0.24(2) 1 d . U P A 2
H8AA H 0.256128 -0.191790 0.344852 0.036 Uiso 0.24(2) 1 calc R . P A 2
H8AB H 0.168844 -0.187895 0.292330 0.036 Uiso 0.24(2) 1 calc R . P A 2
C14A C 0.449(3) -0.074(2) 0.3185(8) 0.021(4) Uani 0.23(2) 1 d . U P A 2
H14A H 0.483305 -0.136037 0.301656 0.025 Uiso 0.23(2) 1 calc R . P A 2
H14B H 0.505251 -0.017196 0.304612 0.025 Uiso 0.23(2) 1 calc R . P A 2
C13A C 0.475(2) -0.082(2) 0.3757(10) 0.023(5) Uani 0.23(2) 1 d . U P A 2
H13A H 0.427551 -0.143225 0.389298 0.027 Uiso 0.23(2) 1 calc R . P A 2
H13B H 0.583278 -0.083814 0.383535 0.027 Uiso 0.23(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N2 1.960(4) . ?
Co1 F2 1.871(2) . ?
Co1 F3 1.871(3) . ?
Co1 F1 1.857(3) . ?
Co1 N3 1.958(4) . ?
Co1 N1 1.960(4) . ?
N2 C8 1.481(6) . ?
N2 C2 1.517(8) . ?
N2 C3 1.486(7) . ?
N2 C8A 1.40(2) . ?
N2 C14A 1.60(2) . ?
N3 C5 1.463(7) . ?
N3 C9 1.480(6) . ?
N3 C4 1.519(7) . ?
N3 C9A 1.63(2) . ?
N3 C13A 1.46(2) . ?
N1 C7 1.473(6) . ?
N1 C6 1.541(9) . ?
N1 C1 1.467(8) . ?
N1 C11A 1.41(2) . ?
N1 C15A 1.67(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.491(15) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.508(12) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.511(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
O1 H1C 0.8495 . ?
O1 H1D 0.8509 . ?
O2 H2C 0.8511 . ?
O2 H2D 0.8506 . ?
O3 H3C 0.8504 . ?
O3 H3D 0.8497 . ?
O4 H4C 0.8505 . ?
O4 H4D 0.8498 . ?
C11A H11A 0.9300 . ?
C11A C9A 1.54(4) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C15A C8A 1.51(5) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C14A C13A 1.52(4) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Co1 N1 87.62(16) . . ?
F2 Co1 N2 178.92(13) . . ?
F2 Co1 F3 89.58(11) . . ?
F2 Co1 N3 92.11(14) . . ?
F2 Co1 N1 91.39(14) . . ?
F3 Co1 N2 90.91(13) . . ?
F3 Co1 N3 178.13(14) . . ?
F3 Co1 N1 92.80(14) . . ?
F1 Co1 N2 91.06(14) . . ?
F1 Co1 F2 89.92(12) . . ?
F1 Co1 F3 88.29(13) . . ?
F1 Co1 N3 90.92(15) . . ?
F1 Co1 N1 178.30(14) . . ?
N3 Co1 N2 87.41(15) . . ?
N3 Co1 N1 87.95(15) . . ?
C8 N2 Co1 113.7(3) . . ?
C8 N2 C2 106.3(5) . . ?
C8 N2 C3 112.9(5) . . ?
C2 N2 Co1 103.2(4) . . ?
C3 N2 Co1 110.1(3) . . ?
C3 N2 C2 110.1(6) . . ?
C8A N2 Co1 114.7(11) . . ?
C8A N2 C14A 109(2) . . ?
C14A N2 Co1 101.3(9) . . ?
C5 N3 Co1 110.5(4) . . ?
C5 N3 C9 113.1(5) . . ?
C5 N3 C4 110.8(7) . . ?
C9 N3 Co1 112.6(3) . . ?
C9 N3 C4 105.5(4) . . ?
C4 N3 Co1 103.9(3) . . ?
C9A N3 Co1 99.2(10) . . ?
C13A N3 Co1 112.4(9) . . ?
C13A N3 C9A 105.6(16) . . ?
C7 N1 Co1 113.6(3) . . ?
C7 N1 C6 106.3(4) . . ?
C6 N1 Co1 102.1(4) . . ?
C1 N1 Co1 109.9(4) . . ?
C1 N1 C7 112.7(4) . . ?
C1 N1 C6 111.7(7) . . ?
C11A N1 Co1 116.0(10) . . ?
C11A N1 C15A 107.3(19) . . ?
C15A N1 Co1 98.6(8) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C2 H2A 109.9 . . ?
N2 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C1 C2 N2 109.0(7) . . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 . . ?
N3 C5 H5A 110.1 . . ?
N3 C5 H5B 110.1 . . ?
N3 C5 C6 108.2(7) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C6 H6A 110.0 . . ?
N1 C6 H6B 110.0 . . ?
C5 C6 N1 108.5(7) . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C4 H4A 110.1 . . ?
N3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.5 . . ?
C3 C4 N3 107.8(6) . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
N2 C3 C4 108.2(6) . . ?
N2 C3 H3A 110.1 . . ?
N2 C3 H3B 110.1 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
N1 C1 C2 109.2(7) . . ?
N1 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
H1C O1 H1D 109.4 . . ?
H2C O2 H2D 109.3 . . ?
H3C O3 H3D 109.5 . . ?
H4C O4 H4D 104.5 . . ?
N1 C11A H11A 128.7 . . ?
N1 C11A C9A 103(2) . . ?
C9A C11A H11A 128.7 . . ?
N3 C9A H9AA 109.5 . . ?
N3 C9A H9AB 109.5 . . ?
C11A C9A N3 110.6(17) . . ?
C11A C9A H9AA 109.5 . . ?
C11A C9A H9AB 109.5 . . ?
H9AA C9A H9AB 108.1 . . ?
N1 C15A H15A 110.3 . . ?
N1 C15A H15B 110.3 . . ?
H15A C15A H15B 108.5 . . ?
C8A C15A N1 107(2) . . ?
C8A C15A H15A 110.3 . . ?
C8A C15A H15B 110.3 . . ?
N2 C8A C15A 105(2) . . ?
N2 C8A H8AA 110.7 . . ?
N2 C8A H8AB 110.7 . . ?
C15A C8A H8AA 110.7 . . ?
C15A C8A H8AB 110.7 . . ?
H8AA C8A H8AB 108.8 . . ?
N2 C14A H14A 110.4 . . ?
N2 C14A H14B 110.4 . . ?
H14A C14A H14B 108.6 . . ?
C13A C14A N2 106.5(17) . . ?
C13A C14A H14A 110.4 . . ?
C13A C14A H14B 110.4 . . ?
N3 C13A C14A 105(2) . . ?
N3 C13A H13A 110.7 . . ?
N3 C13A H13B 110.7 . . ?
C14A C13A H13A 110.7 . . ?
C14A C13A H13B 110.7 . . ?
H13A C13A H13B 108.8 . . ?

_olex2_exptl_crystal_mounting_method MiTegen
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.447
_oxdiff_exptl_absorpt_empirical_full_min 0.785
####################################################################### 
# 
# 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_2018fmm8148-39r
_database_code_depnum_ccdc_archive 'CCDC 1897030'
loop_
_audit_author_name
_audit_author_address
'Francesco Monzittu'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2019-02-13 deposited with the CCDC.	2019-03-19 downloaded from the CCDC.
;
_audit_creation_date             2018-08-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H25 F3 Fe N3, 2(H2 O)'
_chemical_formula_sum            'C15 H29 F3 Fe N3 O2'
_chemical_formula_weight         396.26
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H27F3N3FeO
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.5216(3)
_cell_length_b                   12.4903(4)
_cell_length_c                   29.8518(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3550.20(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    14028
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.5120
_cell_measurement_theta_min      2.2010
_shelx_estimated_absorpt_T_max   0.987
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            74969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.767
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  61.00   0.50    5.00    --    5.00 -19.00  60.00  290
  2  ω    -96.00  24.00   0.50    5.00    --   -6.30 -57.00 -90.00  240
  3  ω    -96.00  28.00   0.50    5.00    --   -6.30 -70.00  60.00  248
  4  ω    -96.00  24.00   0.50    5.00    --   -6.30 -57.00-180.00  240
  5  ω    -84.00 -59.00   0.50    5.00    --    5.00 -38.00 -30.00   50
  6  ω    -37.00  83.00   0.50    5.00    --   -6.30  57.00-120.00  240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0737634000
_diffrn_orient_matrix_UB_12      -0.0060118000
_diffrn_orient_matrix_UB_13      0.0021905000
_diffrn_orient_matrix_UB_21      0.0101537000
_diffrn_orient_matrix_UB_22      0.0506749000
_diffrn_orient_matrix_UB_23      -0.0102407000
_diffrn_orient_matrix_UB_31      -0.0027735000
_diffrn_orient_matrix_UB_32      0.0249193000
_diffrn_orient_matrix_UB_33      0.0213186000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6541
_reflns_number_total             6982
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 2621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0298
_refine_ls_restrained_S_all      1.070
_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)+(0.0172P)²+1.5907P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0573
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4C,H4D), O3(H3C,H3D), O1(H1C,H1D), O2(H2C,H2D)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C23(H23A,H23B), C18(H18A,H18B), C3(H3A,H3B), C8(H8A,H8B), C2(H2A,
 H2B), C20(H20A,H20B), C21(H21A,H21B), C5(H5A,H5B), C16(H16A,H16B), C4(H4A,H4B),
  C1(H1A,H1B), C19(H19A,H19B), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C28(H28), C14(H14), C12(H12), C27(H27), C11(H11), C26(H26),
 C10(H10), C29(H29), C13(H13)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C)
;
_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
Fe1 Fe 0.65535(4) 0.45367(3) 0.43117(2) 0.00977(10) Uani 1 1 d . . . . .
Fe2 Fe 0.40454(5) 0.46570(4) 0.18827(2) 0.01114(10) Uani 1 1 d . . . . .
F1 F 0.8266(2) 0.40800(14) 0.45669(6) 0.0151(4) Uani 1 1 d . . . . .
F2 F 0.6771(2) 0.39569(14) 0.37393(6) 0.0146(4) Uani 1 1 d . . . . .
F6 F 0.2807(2) 0.35545(15) 0.20285(6) 0.0200(4) Uani 1 1 d . . . . .
F5 F 0.4987(2) 0.40201(14) 0.13932(6) 0.0160(4) Uani 1 1 d . . . . .
F3 F 0.5445(2) 0.34568(15) 0.45695(6) 0.0182(4) Uani 1 1 d . . . . .
F4 F 0.5387(2) 0.43828(15) 0.23296(6) 0.0197(4) Uani 1 1 d . . . . .
O4 O 0.5192(3) 0.37576(18) 0.04949(8) 0.0211(5) Uani 1 1 d . . . . .
H4C H 0.517459 0.393695 0.076986 0.032 Uiso 1 1 d G . . . .
H4D H 0.478449 0.426929 0.035977 0.032 Uiso 1 1 d G . . . .
O3 O 0.7681(3) 0.4294(2) 0.28538(8) 0.0278(6) Uani 1 1 d . . . . .
H3C H 0.692315 0.430760 0.270300 0.042 Uiso 1 1 d G . . . .
H3D H 0.741820 0.416334 0.312010 0.042 Uiso 1 1 d G . . . .
O1 O 1.0875(3) 0.4613(2) 0.49402(9) 0.0321(6) Uani 1 1 d . . . . .
H1C H 1.014043 0.436113 0.481778 0.048 Uiso 1 1 d G . . . .
H1D H 1.139955 0.407074 0.498135 0.048 Uiso 1 1 d G . . . .
N4 N 0.3006(3) 0.5802(2) 0.23430(8) 0.0137(6) Uani 1 1 d . . . . .
O2 O 0.3022(3) 0.3052(2) 0.50396(9) 0.0274(6) Uani 1 1 d . . . . .
H2C H 0.377308 0.308374 0.488678 0.041 Uiso 1 1 d G . . . .
H2D H 0.303003 0.243050 0.515529 0.041 Uiso 1 1 d G . . . .
N1 N 0.6113(3) 0.5573(2) 0.48933(8) 0.0114(5) Uani 1 1 d . . . . .
N2 N 0.7561(3) 0.6068(2) 0.40939(8) 0.0105(5) Uani 1 1 d . . . . .
N3 N 0.4699(3) 0.5409(2) 0.40699(8) 0.0123(5) Uani 1 1 d . . . . .
N6 N 0.2473(3) 0.5379(2) 0.14295(8) 0.0120(5) Uani 1 1 d . . . . .
N5 N 0.5111(3) 0.6206(2) 0.17057(8) 0.0107(5) Uani 1 1 d . . . . .
C6 C 0.4563(3) 0.5696(3) 0.48879(10) 0.0133(7) Uani 1 1 d . . . . .
H6A H 0.427763 0.622227 0.511845 0.016 Uiso 1 1 calc R . . . .
H6B H 0.411708 0.500141 0.496155 0.016 Uiso 1 1 calc R . . . .
C23 C 0.6640(4) 0.5967(2) 0.17334(10) 0.0134(7) Uani 1 1 d . . . . .
H23A H 0.681971 0.530186 0.156212 0.016 Uiso 1 1 calc R . . . .
H23B H 0.687120 0.581586 0.205058 0.016 Uiso 1 1 calc R . . . .
C18 C 0.4634(3) 0.6415(3) 0.12388(10) 0.0125(7) Uani 1 1 d . . . . .
H18A H 0.504535 0.587412 0.103505 0.015 Uiso 1 1 calc R . . . .
H18B H 0.496354 0.713014 0.114201 0.015 Uiso 1 1 calc R . . . .
C9 C 0.9723(3) 0.6695(2) 0.36459(10) 0.0117(6) Uani 1 1 d . . . . .
C25 C 0.8348(3) 0.7496(2) 0.18621(11) 0.0146(6) Uani 1 1 d . . . . .
H25 H 0.809532 0.750191 0.216995 0.018 Uiso 1 1 calc R . . . .
C28 C 0.9058(4) 0.7516(3) 0.09613(11) 0.0178(7) Uani 1 1 d . . . . .
H28 H 0.928830 0.753318 0.065178 0.021 Uiso 1 1 calc R . . . .
C14 C 0.9574(4) 0.7095(3) 0.32137(10) 0.0151(7) Uani 1 1 d . . . . .
H14 H 0.882890 0.684636 0.302939 0.018 Uiso 1 1 calc R . . . .
C15 C 0.3653(3) 0.4639(3) 0.38965(10) 0.0172(7) Uani 1 1 d . . . . .
H15A H 0.408730 0.419249 0.366485 0.026 Uiso 1 1 calc GR . . . .
H15B H 0.285774 0.503072 0.376772 0.026 Uiso 1 1 calc GR . . . .
H15C H 0.332080 0.418387 0.414193 0.026 Uiso 1 1 calc GR . . . .
C12 C 1.1595(4) 0.8220(3) 0.33092(11) 0.0189(7) Uani 1 1 d . . . . .
H12 H 1.224321 0.872633 0.319225 0.023 Uiso 1 1 calc R . . . .
C27 C 0.9783(4) 0.8153(3) 0.12609(12) 0.0180(7) Uani 1 1 d . . . . .
H27 H 1.053923 0.858514 0.115880 0.022 Uiso 1 1 calc R . . . .
C3 C 0.6518(4) 0.6747(2) 0.38494(10) 0.0127(6) Uani 1 1 d . . . . .
H3A H 0.697424 0.707760 0.358559 0.015 Uiso 1 1 calc R . . . .
H3B H 0.619032 0.732950 0.404863 0.015 Uiso 1 1 calc R . . . .
C24 C 0.7646(3) 0.6817(2) 0.15660(10) 0.0124(6) Uani 1 1 d . . . . .
C8 C 0.8799(3) 0.5792(2) 0.38072(10) 0.0115(7) Uani 1 1 d . . . . .
H8A H 0.844687 0.540483 0.354053 0.014 Uiso 1 1 calc R . . . .
H8B H 0.939568 0.528621 0.397730 0.014 Uiso 1 1 calc R . . . .
C11 C 1.1748(4) 0.7846(3) 0.37434(11) 0.0188(7) Uani 1 1 d . . . . .
H11 H 1.248728 0.810634 0.392717 0.023 Uiso 1 1 calc R . . . .
C26 C 0.9412(3) 0.8163(3) 0.17105(11) 0.0161(7) Uani 1 1 d . . . . .
H26 H 0.988509 0.862428 0.191362 0.019 Uiso 1 1 calc R . . . .
C10 C 1.0812(4) 0.7085(3) 0.39094(11) 0.0163(7) Uani 1 1 d . . . . .
H10 H 1.092085 0.682846 0.420702 0.020 Uiso 1 1 calc R . . . .
C2 C 0.8029(3) 0.6573(3) 0.45176(10) 0.0130(7) Uani 1 1 d . . . . .
H2A H 0.837445 0.730566 0.445495 0.016 Uiso 1 1 calc R . . . .
H2B H 0.881507 0.615488 0.464566 0.016 Uiso 1 1 calc R . . . .
C20 C 0.1278(3) 0.5625(3) 0.17300(10) 0.0142(7) Uani 1 1 d . . . . .
H20A H 0.085236 0.494705 0.183554 0.017 Uiso 1 1 calc R . . . .
H20B H 0.055406 0.602480 0.156093 0.017 Uiso 1 1 calc R . . . .
C21 C 0.1739(3) 0.6281(3) 0.21298(10) 0.0146(7) Uani 1 1 d . . . . .
H21A H 0.195365 0.702060 0.203241 0.018 Uiso 1 1 calc R . . . .
H21B H 0.096650 0.631400 0.235120 0.018 Uiso 1 1 calc R . . . .
C7 C 0.6542(4) 0.5011(3) 0.53076(10) 0.0166(7) Uani 1 1 d . . . . .
H7A H 0.612760 0.429297 0.531170 0.025 Uiso 1 1 calc GR . . . .
H7B H 0.621502 0.541505 0.556899 0.025 Uiso 1 1 calc GR . . . .
H7C H 0.756820 0.495286 0.531658 0.025 Uiso 1 1 calc GR . . . .
C29 C 0.7996(3) 0.6855(3) 0.11128(11) 0.0158(7) Uani 1 1 d . . . . .
H29 H 0.749704 0.642077 0.090547 0.019 Uiso 1 1 calc R . . . .
C13 C 1.0509(4) 0.7860(3) 0.30485(11) 0.0176(7) Uani 1 1 d . . . . .
H13 H 1.039145 0.813205 0.275367 0.021 Uiso 1 1 calc R . . . .
C5 C 0.4062(4) 0.6068(3) 0.44321(10) 0.0146(7) Uani 1 1 d . . . . .
H5A H 0.302560 0.601284 0.441676 0.018 Uiso 1 1 calc R . . . .
H5B H 0.432140 0.682890 0.438872 0.018 Uiso 1 1 calc R . . . .
C16 C 0.4088(4) 0.6624(3) 0.24472(10) 0.0160(7) Uani 1 1 d . . . . .
H16A H 0.484623 0.629650 0.262805 0.019 Uiso 1 1 calc R . . . .
H16B H 0.365940 0.720627 0.262591 0.019 Uiso 1 1 calc R . . . .
C22 C 0.2606(4) 0.5225(3) 0.27570(10) 0.0211(8) Uani 1 1 d . . . . .
H22A H 0.188870 0.468772 0.268648 0.032 Uiso 1 1 calc GR . . . .
H22B H 0.222931 0.573491 0.297563 0.032 Uiso 1 1 calc GR . . . .
H22C H 0.343430 0.486967 0.288285 0.032 Uiso 1 1 calc GR . . . .
C4 C 0.5265(3) 0.6085(3) 0.36967(10) 0.0138(7) Uani 1 1 d . . . . .
H4A H 0.451663 0.656971 0.358721 0.017 Uiso 1 1 calc R . . . .
H4B H 0.555197 0.561793 0.344500 0.017 Uiso 1 1 calc R . . . .
C30 C 0.1996(3) 0.4599(3) 0.10901(10) 0.0173(7) Uani 1 1 d . . . . .
H30A H 0.276010 0.445812 0.087830 0.026 Uiso 1 1 calc GR . . . .
H30B H 0.118656 0.489211 0.092847 0.026 Uiso 1 1 calc GR . . . .
H30C H 0.172497 0.393059 0.123839 0.026 Uiso 1 1 calc GR . . . .
C1 C 0.6837(3) 0.6628(2) 0.48557(10) 0.0133(7) Uani 1 1 d . . . . .
H1A H 0.721596 0.683681 0.515202 0.016 Uiso 1 1 calc R . . . .
H1B H 0.615356 0.718123 0.476142 0.016 Uiso 1 1 calc R . . . .
C19 C 0.3038(3) 0.6369(2) 0.12102(10) 0.0131(7) Uani 1 1 d . . . . .
H19A H 0.263484 0.700802 0.135804 0.016 Uiso 1 1 calc R . . . .
H19B H 0.274847 0.637966 0.089175 0.016 Uiso 1 1 calc R . . . .
C17 C 0.4705(3) 0.7086(2) 0.20188(10) 0.0132(7) Uani 1 1 d . . . . .
H17A H 0.400447 0.755626 0.187274 0.016 Uiso 1 1 calc R . . . .
H17B H 0.554126 0.752348 0.209169 0.016 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 F1 1.8878(19) . ?
Fe1 F2 1.8673(17) . ?
Fe1 F3 1.8778(19) . ?
Fe1 N1 2.206(2) . ?
Fe1 N2 2.237(3) . ?
Fe1 N3 2.197(3) . ?
Fe2 F6 1.8646(19) . ?
Fe2 F5 1.8901(18) . ?
Fe2 F4 1.8784(18) . ?
Fe2 N4 2.217(3) . ?
Fe2 N6 2.211(2) . ?
Fe2 N5 2.248(3) . ?
O4 H4C 0.8511 . ?
O4 H4D 0.8497 . ?
O3 H3C 0.8503 . ?
O3 H3D 0.8490 . ?
O1 H1C 0.8493 . ?
O1 H1D 0.8505 . ?
N4 C21 1.489(4) . ?
N4 C16 1.488(4) . ?
N4 C22 1.481(4) . ?
O2 H2C 0.8495 . ?
O2 H2D 0.8501 . ?
N1 C6 1.484(4) . ?
N1 C7 1.480(4) . ?
N1 C1 1.492(4) . ?
N2 C3 1.496(4) . ?
N2 C8 1.497(4) . ?
N2 C2 1.482(4) . ?
N3 C15 1.478(4) . ?
N3 C5 1.488(4) . ?
N3 C4 1.498(4) . ?
N6 C20 1.480(4) . ?
N6 C30 1.477(4) . ?
N6 C19 1.498(4) . ?
N5 C23 1.489(4) . ?
N5 C18 1.489(4) . ?
N5 C17 1.494(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.515(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.515(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.523(5) . ?
C9 C14 1.391(4) . ?
C9 C8 1.509(4) . ?
C9 C10 1.390(5) . ?
C25 H25 0.9500 . ?
C25 C24 1.396(4) . ?
C25 C26 1.387(5) . ?
C28 H28 0.9500 . ?
C28 C27 1.382(5) . ?
C28 C29 1.382(5) . ?
C14 H14 0.9500 . ?
C14 C13 1.396(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C11 1.386(5) . ?
C12 C13 1.370(5) . ?
C27 H27 0.9500 . ?
C27 C26 1.388(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.521(5) . ?
C24 C29 1.394(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C11 H11 0.9500 . ?
C11 C10 1.394(5) . ?
C26 H26 0.9500 . ?
C10 H10 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.520(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.513(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C29 H29 0.9500 . ?
C13 H13 0.9500 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.521(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?

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
F1 Fe1 N1 91.36(9) . . ?
F1 Fe1 N2 90.30(9) . . ?
F1 Fe1 N3 167.58(9) . . ?
F2 Fe1 F1 99.00(8) . . ?
F2 Fe1 F3 99.13(8) . . ?
F2 Fe1 N1 165.67(8) . . ?
F2 Fe1 N2 91.04(8) . . ?
F2 Fe1 N3 88.90(9) . . ?
F3 Fe1 F1 95.91(8) . . ?
F3 Fe1 N1 89.55(9) . . ?
F3 Fe1 N2 167.08(9) . . ?
F3 Fe1 N3 92.25(9) . . ?
N1 Fe1 N2 78.96(9) . . ?
N3 Fe1 N1 79.32(9) . . ?
N3 Fe1 N2 79.92(10) . . ?
F6 Fe2 F5 99.77(8) . . ?
F6 Fe2 F4 97.47(8) . . ?
F6 Fe2 N4 92.83(9) . . ?
F6 Fe2 N6 90.90(9) . . ?
F6 Fe2 N5 167.45(9) . . ?
F5 Fe2 N4 164.29(9) . . ?
F5 Fe2 N6 91.14(8) . . ?
F5 Fe2 N5 88.07(9) . . ?
F4 Fe2 F5 98.61(8) . . ?
F4 Fe2 N4 88.92(9) . . ?
F4 Fe2 N6 165.85(9) . . ?
F4 Fe2 N5 90.96(9) . . ?
N4 Fe2 N5 77.99(9) . . ?
N6 Fe2 N4 79.25(9) . . ?
N6 Fe2 N5 79.08(10) . . ?
H4C O4 H4D 104.5 . . ?
H3C O3 H3D 104.5 . . ?
H1C O1 H1D 104.5 . . ?
C21 N4 Fe2 110.84(18) . . ?
C16 N4 Fe2 105.40(19) . . ?
C16 N4 C21 111.9(2) . . ?
C22 N4 Fe2 108.5(2) . . ?
C22 N4 C21 110.1(3) . . ?
C22 N4 C16 109.9(2) . . ?
H2C O2 H2D 104.6 . . ?
C6 N1 Fe1 103.95(18) . . ?
C6 N1 C1 111.6(2) . . ?
C7 N1 Fe1 109.08(18) . . ?
C7 N1 C6 109.4(2) . . ?
C7 N1 C1 110.8(2) . . ?
C1 N1 Fe1 111.80(18) . . ?
C3 N2 Fe1 109.96(19) . . ?
C3 N2 C8 112.0(2) . . ?
C8 N2 Fe1 107.88(18) . . ?
C2 N2 Fe1 104.17(17) . . ?
C2 N2 C3 112.0(2) . . ?
C2 N2 C8 110.5(2) . . ?
C15 N3 Fe1 109.5(2) . . ?
C15 N3 C5 109.9(2) . . ?
C15 N3 C4 110.4(2) . . ?
C5 N3 Fe1 111.31(18) . . ?
C5 N3 C4 112.0(3) . . ?
C4 N3 Fe1 103.59(18) . . ?
C20 N6 Fe2 103.54(17) . . ?
C20 N6 C19 111.7(2) . . ?
C30 N6 Fe2 111.02(19) . . ?
C30 N6 C20 108.4(2) . . ?
C30 N6 C19 110.8(2) . . ?
C19 N6 Fe2 111.13(18) . . ?
C23 N5 Fe2 104.81(18) . . ?
C23 N5 C18 112.7(2) . . ?
C23 N5 C17 111.5(2) . . ?
C18 N5 Fe2 103.48(18) . . ?
C18 N5 C17 112.2(2) . . ?
C17 N5 Fe2 111.68(18) . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 C5 110.8(2) . . ?
H6A C6 H6B 108.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
N5 C23 H23A 108.0 . . ?
N5 C23 H23B 108.0 . . ?
N5 C23 C24 117.3(3) . . ?
H23A C23 H23B 107.2 . . ?
C24 C23 H23A 108.0 . . ?
C24 C23 H23B 108.0 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
N5 C18 C19 110.5(3) . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C14 C9 C8 120.3(3) . . ?
C10 C9 C14 118.4(3) . . ?
C10 C9 C8 121.1(3) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C26 C25 C24 120.5(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C29 C28 C27 119.9(3) . . ?
C9 C14 H14 119.7 . . ?
C9 C14 C13 120.6(3) . . ?
C13 C14 H14 119.7 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C13 C12 C11 120.0(3) . . ?
C28 C27 H27 119.9 . . ?
C28 C27 C26 120.2(3) . . ?
C26 C27 H27 119.9 . . ?
N2 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
N2 C3 C4 111.1(2) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C25 C24 C23 121.3(3) . . ?
C29 C24 C23 119.7(3) . . ?
C29 C24 C25 118.7(3) . . ?
N2 C8 C9 118.0(2) . . ?
N2 C8 H8A 107.8 . . ?
N2 C8 H8B 107.8 . . ?
C9 C8 H8A 107.8 . . ?
C9 C8 H8B 107.8 . . ?
H8A C8 H8B 107.1 . . ?
C12 C11 H11 120.1 . . ?
C12 C11 C10 119.7(3) . . ?
C10 C11 H11 120.1 . . ?
C25 C26 C27 119.7(3) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C9 C10 C11 121.0(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
N2 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
N2 C2 C1 111.2(3) . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
N6 C20 H20A 109.3 . . ?
N6 C20 H20B 109.3 . . ?
N6 C20 C21 111.5(2) . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
N4 C21 C20 110.8(3) . . ?
N4 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C28 C29 C24 120.8(3) . . ?
C28 C29 H29 119.6 . . ?
C24 C29 H29 119.6 . . ?
C14 C13 H13 119.8 . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H13 119.8 . . ?
N3 C5 C6 110.7(2) . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
N4 C16 C17 110.7(2) . . ?
H16A C16 H16B 108.1 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C4 C3 111.4(2) . . ?
N3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
N6 C30 H30A 109.5 . . ?
N6 C30 H30B 109.5 . . ?
N6 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C1 C2 110.8(2) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N6 C19 C18 111.4(3) . . ?
N6 C19 H19A 109.3 . . ?
N6 C19 H19B 109.3 . . ?
C18 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
N5 C17 C16 110.3(3) . . ?
N5 C17 H17A 109.6 . . ?
N5 C17 H17B 109.6 . . ?
C16 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?

_olex2_exptl_crystal_mounting_method MiTeGen
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.719
####################################################################### 
# 
# 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_2018fmmtmfefter
_database_code_depnum_ccdc_archive 'CCDC 1860122'
loop_
_audit_author_name
_audit_author_address
'Francesco Monzittu'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2018-08-03 deposited with the CCDC.	2019-03-19 downloaded from the CCDC.
;
_audit_creation_date             2018-03-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H11 F3 Fe N3, 3(H2 O)'
_chemical_formula_sum            'C15 H17 F3 Fe N3 O3'
_chemical_formula_weight         400.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H11N3F3Fe
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.6981(2)
_cell_length_b                   25.5075(5)
_cell_length_c                   7.4413(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.155(2)
_cell_angle_gamma                90
_cell_volume                     1613.96(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19525
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.0170
_cell_measurement_theta_min      2.3740
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.930
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            34245
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.395
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00  20.00   0.50    1.00    --  -17.30 -57.00  90.00  254
  2  ω    -55.00  72.00   0.50    1.00    --  -17.30  57.00  90.00  254
  3  ω   -107.00  23.00   0.50    1.00    --  -17.30 -70.00  60.00  260
  4  ω   -107.00  72.00   0.50    1.00    --  -17.30   0.00  60.00  358
  5  ω    -55.00  72.00   0.50    1.00    --  -17.30  57.00  30.00  254
  6  ω   -107.00  23.00   0.50    1.00    --  -17.30 -70.00 -90.00  260
  7  ω    -58.00  20.00   0.50    1.00    --  -17.30  70.00-120.00  156
  8  ω    -55.00  72.00   0.50    1.00    --  -17.30  57.00-180.00  254
;
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0799396000
_diffrn_orient_matrix_UB_12      -0.0050763000
_diffrn_orient_matrix_UB_13      -0.0406901000
_diffrn_orient_matrix_UB_21      0.0129525000
_diffrn_orient_matrix_UB_22      -0.0272210000
_diffrn_orient_matrix_UB_23      0.0159386000
_diffrn_orient_matrix_UB_31      -0.0200074000
_diffrn_orient_matrix_UB_32      0.0026021000
_diffrn_orient_matrix_UB_33      0.0871530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2971
_reflns_number_total             3177
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0206
_refine_ls_restrained_S_all      1.062
_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)+(0.0286P)²+0.9964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0583
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O3(H3A,H3B), O2(H2A,H2B), O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C9(H9), C15(H15), C12(H12), C8(H8), C14(H14), C4(H4),
 C1(H1), C3(H3), C2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.79324(2) 0.61892(2) 0.66293(3) 0.00973(7) Uani 1 1 d . . . . .
F3 F 0.89858(10) 0.62285(3) 0.91457(11) 0.01588(18) Uani 1 1 d . . . . .
F1 F 0.68624(10) 0.61058(3) 0.41777(11) 0.01643(18) Uani 1 1 d . . . . .
F2 F 0.97921(10) 0.63427(3) 0.58911(12) 0.01938(19) Uani 1 1 d . . . . .
O3 O 1.10691(13) 0.70018(4) 1.04260(14) 0.0201(2) Uani 1 1 d . . . . .
H3A H 1.043098 0.675781 0.999832 0.030 Uiso 1 1 d G . . . .
H3B H 1.116985 0.697963 1.158460 0.030 Uiso 1 1 d G . . . .
O2 O 1.15066(13) 0.70044(4) 0.41740(15) 0.0209(2) Uani 1 1 d . . . . .
H2A H 1.095973 0.679606 0.467764 0.031 Uiso 1 1 d G . . . .
H2B H 1.131956 0.730586 0.456265 0.031 Uiso 1 1 d G . . . .
O1 O 0.77722(13) 0.55856(4) 0.14711(15) 0.0218(2) Uani 1 1 d . . . . .
H1A H 0.754371 0.578096 0.230088 0.033 Uiso 1 1 d G . . . .
H1B H 0.823562 0.576470 0.078279 0.033 Uiso 1 1 d G . . . .
N3 N 0.70113(13) 0.69609(4) 0.68189(15) 0.0117(2) Uani 1 1 d . . . . .
N2 N 0.57362(13) 0.60786(4) 0.73663(15) 0.0110(2) Uani 1 1 d . . . . .
N1 N 0.77265(13) 0.53544(4) 0.69694(15) 0.0123(2) Uani 1 1 d . . . . .
C5 C 0.63354(16) 0.51780(5) 0.72688(18) 0.0122(3) Uani 1 1 d . . . . .
C11 C 0.55773(16) 0.70009(5) 0.72322(18) 0.0122(3) Uani 1 1 d . . . . .
C10 C 0.48581(16) 0.64959(5) 0.75715(18) 0.0122(3) Uani 1 1 d . . . . .
C13 C 0.56882(17) 0.79330(6) 0.70862(19) 0.0165(3) Uani 1 1 d . . . . .
H13 H 0.523178 0.826805 0.717045 0.020 Uiso 1 1 calc R . . . .
C7 C 0.38103(16) 0.55057(6) 0.81011(19) 0.0152(3) Uani 1 1 d . . . . .
H7 H 0.346162 0.516002 0.827357 0.018 Uiso 1 1 calc R . . . .
C6 C 0.52370(16) 0.55926(5) 0.75947(18) 0.0123(3) Uani 1 1 d . . . . .
C9 C 0.34210(16) 0.64383(6) 0.80753(19) 0.0157(3) Uani 1 1 d . . . . .
H9 H 0.280331 0.673551 0.822943 0.019 Uiso 1 1 calc R . . . .
C15 C 0.77846(16) 0.73981(6) 0.65560(18) 0.0139(3) Uani 1 1 d . . . . .
H15 H 0.879324 0.736777 0.626511 0.017 Uiso 1 1 calc R . . . .
C12 C 0.48761(17) 0.74842(6) 0.73565(19) 0.0146(3) Uani 1 1 d . . . . .
H12 H 0.385664 0.750626 0.762244 0.018 Uiso 1 1 calc R . . . .
C8 C 0.29102(16) 0.59367(6) 0.83476(19) 0.0166(3) Uani 1 1 d . . . . .
H8 H 0.193452 0.588774 0.870634 0.020 Uiso 1 1 calc R . . . .
C14 C 0.71676(17) 0.78922(6) 0.66926(19) 0.0163(3) Uani 1 1 d . . . . .
H14 H 0.774719 0.819706 0.651987 0.020 Uiso 1 1 calc R . . . .
C4 C 0.59809(17) 0.46502(6) 0.72374(19) 0.0159(3) Uani 1 1 d . . . . .
H4 H 0.499651 0.453398 0.744866 0.019 Uiso 1 1 calc R . . . .
C1 C 0.87995(17) 0.50052(6) 0.6703(2) 0.0161(3) Uani 1 1 d . . . . .
H1 H 0.979393 0.512878 0.654944 0.019 Uiso 1 1 calc R . . . .
C3 C 0.70821(18) 0.42927(6) 0.6893(2) 0.0180(3) Uani 1 1 d . . . . .
H3 H 0.684915 0.392842 0.683000 0.022 Uiso 1 1 calc R . . . .
C2 C 0.85235(18) 0.44707(6) 0.6643(2) 0.0184(3) Uani 1 1 d . . . . .
H2 H 0.930545 0.423180 0.643384 0.022 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 F3 1.9062(8) . ?
Fe1 F1 1.8774(8) . ?
Fe1 F2 1.8563(8) . ?
Fe1 N3 2.1410(11) . ?
Fe1 N2 2.1144(12) . ?
Fe1 N1 2.1564(12) . ?
O3 H3A 0.8499 . ?
O3 H3B 0.8499 . ?
O2 H2A 0.8509 . ?
O2 H2B 0.8493 . ?
O1 H1A 0.8490 . ?
O1 H1B 0.8488 . ?
N3 C11 1.3499(18) . ?
N3 C15 1.3377(18) . ?
N2 C10 1.3374(18) . ?
N2 C6 1.3361(18) . ?
N1 C5 1.3527(18) . ?
N1 C1 1.3347(18) . ?
C5 C6 1.4792(19) . ?
C5 C4 1.380(2) . ?
C11 C10 1.4768(19) . ?
C11 C12 1.3870(19) . ?
C10 C9 1.386(2) . ?
C13 H13 0.9500 . ?
C13 C12 1.382(2) . ?
C13 C14 1.383(2) . ?
C7 H7 0.9500 . ?
C7 C6 1.389(2) . ?
C7 C8 1.384(2) . ?
C9 H9 0.9500 . ?
C9 C8 1.383(2) . ?
C15 H15 0.9500 . ?
C15 C14 1.382(2) . ?
C12 H12 0.9500 . ?
C8 H8 0.9500 . ?
C14 H14 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.385(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.383(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.382(2) . ?
C2 H2 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 Fe1 N3 89.78(4) . . ?
F3 Fe1 N2 91.48(4) . . ?
F3 Fe1 N1 88.35(4) . . ?
F1 Fe1 F3 176.33(4) . . ?
F1 Fe1 N3 93.01(4) . . ?
F1 Fe1 N2 86.95(4) . . ?
F1 Fe1 N1 88.03(4) . . ?
F2 Fe1 F3 90.63(4) . . ?
F2 Fe1 F1 91.20(4) . . ?
F2 Fe1 N3 100.79(4) . . ?
F2 Fe1 N2 174.92(4) . . ?
F2 Fe1 N1 110.00(4) . . ?
N3 Fe1 N1 149.17(4) . . ?
N2 Fe1 N3 74.60(4) . . ?
N2 Fe1 N1 74.69(4) . . ?
H3A O3 H3B 104.5 . . ?
H2A O2 H2B 104.5 . . ?
H1A O1 H1B 109.7 . . ?
C11 N3 Fe1 117.45(9) . . ?
C15 N3 Fe1 123.37(9) . . ?
C15 N3 C11 119.18(12) . . ?
C10 N2 Fe1 119.49(9) . . ?
C6 N2 Fe1 119.50(9) . . ?
C6 N2 C10 121.01(12) . . ?
C5 N1 Fe1 116.56(9) . . ?
C1 N1 Fe1 124.31(10) . . ?
C1 N1 C5 118.69(12) . . ?
N1 C5 C6 114.85(12) . . ?
N1 C5 C4 121.74(13) . . ?
C4 C5 C6 123.41(13) . . ?
N3 C11 C10 114.71(12) . . ?
N3 C11 C12 121.51(13) . . ?
C12 C11 C10 123.76(13) . . ?
N2 C10 C11 113.70(12) . . ?
N2 C10 C9 121.04(13) . . ?
C9 C10 C11 125.25(13) . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.71(13) . . ?
C14 C13 H13 120.1 . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
C8 C7 C6 118.16(13) . . ?
N2 C6 C5 113.84(12) . . ?
N2 C6 C7 121.04(13) . . ?
C7 C6 C5 125.12(13) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 C10 118.25(13) . . ?
C8 C9 H9 120.9 . . ?
N3 C15 H15 118.8 . . ?
N3 C15 C14 122.31(13) . . ?
C14 C15 H15 118.8 . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.76(13) . . ?
C13 C12 H12 120.6 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.47(13) . . ?
C9 C8 H8 119.8 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.51(13) . . ?
C15 C14 H14 120.7 . . ?
C5 C4 H4 120.5 . . ?
C5 C4 C3 118.99(13) . . ?
C3 C4 H4 120.5 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.73(14) . . ?
C2 C1 H1 118.6 . . ?
C4 C3 H3 120.3 . . ?
C2 C3 C4 119.39(13) . . ?
C2 C3 H3 120.3 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.38(14) . . ?
C3 C2 H2 120.8 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.029
_oxdiff_exptl_absorpt_empirical_full_min 0.615
