# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_CCP-2_HS
_database_code_depnum_ccdc_archive 'CCDC 1439096'
_audit_update_record             
;
2016-10-13 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;
_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H60 Fe2 N48), 2(B1 F4)'
_chemical_formula_sum            'C30 H30 B2 F8 Fe N24'
_chemical_formula_weight         956.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 N3 O3 H25 cl'
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'
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'

_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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'

_cell_length_a                   10.4852(10)
_cell_length_b                   10.4852(10)
_cell_length_c                   23.308(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2219.2(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    248
_cell_measurement_temperature    240.00(14)
_cell_measurement_theta_max      16.8120
_cell_measurement_theta_min      3.9740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_unetI/netI     0.2445
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            1400
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.844
_diffrn_reflns_v_R_equivalents   ?
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  67.00   1.00   70.00    --   15.51  38.00  30.00   71
  2  ω    -17.00  22.00   1.00   70.00    --   15.51 -77.00 -90.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026230000
_diffrn_orient_matrix_UB_12      -0.0670594000
_diffrn_orient_matrix_UB_13      -0.0070258000
_diffrn_orient_matrix_UB_21      0.0678509000
_diffrn_orient_matrix_UB_22      0.0395742000
_diffrn_orient_matrix_UB_23      -0.0149704000
_diffrn_orient_matrix_UB_31      0.0388104000
_diffrn_orient_matrix_UB_32      0.0048019000
_diffrn_orient_matrix_UB_33      0.0255336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                608
_reflns_number_total             1400
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 _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 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_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         1.200
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1400
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.2252
_refine_ls_R_factor_gt           0.1085
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1104P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.3038
_refine_special_details          'Refined as a 2-component twin., Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.620(8) 0.380(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 F2A-F1A
 2 with sigma of 0.02
 C1-C1_$1 \\sim C4_$1-C1_$1 \\sim C4_$1-C2_$1 \\sim C2-C2_$1 \\sim C4-C2 \\sim
C4-C1
 with sigma of 0.002
 F1-B0AA \\sim F2-B0AA
 with sigma of 0.002
 F2A-B0AA \\sim F1-B0AA \\sim F1A-B0AA \\sim F2-B0AA
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F2A \\sim F1A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 C2, C4, C1, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, C8, N3, N7, N13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2A, F1, F1A, B0AA, F2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Others
 Sof(F1A)=1-FVAR(1)
 Sof(F2A)=0.33333*(1-FVAR(2))
 Sof(F2)=0.33333*FVAR(2)
 Sof(F1)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
7.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C1(H1), C2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.0000 0.0000 0.5000 0.0367(10) Uani 1 6 d S T P . .
N14 N -0.1423(9) -0.1858(9) 0.5527(3) 0.041(2) Uani 1 1 d . U . . .
N3 N -0.3230(9) -0.3513(9) 0.6017(3) 0.046(2) Uani 1 1 d . U . . .
N7 N -0.2034(12) -0.3578(11) 0.6172(4) 0.075(3) Uani 1 1 d . U . . .
C8 C -0.2881(12) -0.2515(10) 0.5621(4) 0.044(3) Uani 1 1 d . U . . .
H8 H -0.3538 -0.2292 0.5433 0.053 Uiso 1 1 calc R . . . .
N13 N -0.0948(10) -0.2563(11) 0.5881(4) 0.066(3) Uani 1 1 d . U . . .
C3 C -0.4690(11) -0.4567(12) 0.6258(4) 0.056(3) Uani 1 1 d . U . . .
H3A H -0.4980 -0.5564 0.6127 0.067 Uiso 1 1 calc R . . . .
H3B H -0.5423 -0.4323 0.6118 0.067 Uiso 1 1 calc R . . . .
C4 C -0.4663(11) -0.4530(8) 0.6900(4) 0.045(3) Uani 1 1 d D U . . .
C1 C -0.4913(13) -0.5743(12) 0.72070(13) 0.066(4) Uani 1 1 d D U . . .
H1 H -0.5088 -0.6598 0.7010 0.079 Uiso 1 1 calc R . . . .
C2 C -0.4427(14) -0.3320(13) 0.72070(13) 0.069(3) Uani 1 1 d D U . . .
H2 H -0.4260 -0.2468 0.7010 0.082 Uiso 1 1 calc R . . . .
F1 F -0.3411(12) -0.5408(10) 0.4996(4) 0.117(4) Uani 0.865(7) 1 d D U . A 1
F2 F -0.3333 -0.6667 0.4338(7) 0.135(4) Uani 0.865(7) 3 d DS TU P A 1
B0AA B -0.3333 -0.6667 0.4927(7) 0.089(9) Uani 1 3 d DS TU P . .
F2A F -0.332(9) -0.535(4) 0.4891(16) 0.127(4) Uani 0.045(2) 1 d D U . A 2
F1A F -0.3333 -0.6667 0.5516(8) 0.130(4) Uani 0.40(2) 3 d DS TU P A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0382(13) 0.0382(13) 0.0337(17) 0.000 0.000 0.0191(7)
N14 0.043(4) 0.037(5) 0.040(4) 0.001(4) -0.003(4) 0.018(4)
N3 0.044(5) 0.048(5) 0.041(4) 0.011(4) 0.000(4) 0.019(4)
N7 0.054(5) 0.081(7) 0.088(6) 0.049(6) 0.008(5) 0.033(5)
C8 0.044(5) 0.047(6) 0.040(5) 0.011(4) 0.001(4) 0.022(5)
N13 0.047(5) 0.072(7) 0.077(6) 0.037(5) 0.006(4) 0.028(4)
C3 0.045(7) 0.060(7) 0.041(4) 0.008(4) 0.002(4) 0.011(6)
C4 0.035(6) 0.056(6) 0.034(4) 0.003(4) -0.001(4) 0.015(5)
C1 0.094(10) 0.055(6) 0.038(5) -0.001(4) 0.002(5) 0.028(6)
C2 0.085(10) 0.073(7) 0.051(6) -0.004(5) -0.010(6) 0.042(7)
F1 0.120(5) 0.111(6) 0.146(8) -0.005(3) 0.003(3) 0.077(4)
F2 0.128(6) 0.128(6) 0.147(9) 0.000 0.000 0.064(3)
B0AA 0.104(13) 0.104(13) 0.060(15) 0.000 0.000 0.052(7)
F2A 0.123(6) 0.120(6) 0.146(8) -0.002(3) 0.001(3) 0.068(4)
F1A 0.122(6) 0.122(6) 0.146(8) 0.000 0.000 0.061(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N14 2.150(8) 9_556 ?
Fe1 N14 2.150(8) . ?
Fe1 N14 2.150(8) 3 ?
Fe1 N14 2.150(8) 7_556 ?
Fe1 N14 2.150(8) 11_556 ?
Fe1 N14 2.150(8) 5 ?
N14 C8 1.343(12) . ?
N14 N13 1.358(10) . ?
N3 N7 1.339(12) . ?
N3 C8 1.303(11) . ?
N3 C3 1.479(12) . ?
N7 N13 1.296(12) . ?
C8 H8 0.9400 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.498(12) . ?
C4 C1 1.366(6) . ?
C4 C2 1.366(6) . ?
C1 C1 1.366(6) 10_557 ?
C1 H1 0.9400 . ?
C2 C2 1.366(6) 10_557 ?
C2 H2 0.9400 . ?
F1 B0AA 1.372(8) . ?
F2 B0AA 1.373(8) . ?
B0AA F1 1.372(8) 5_545 ?
B0AA F1 1.372(8) 3_445 ?
B0AA F2A 1.373(8) . ?
B0AA F2A 1.373(8) 3_445 ?
B0AA F2A 1.373(8) 5_545 ?
B0AA F1A 1.373(8) . ?

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
N14 Fe1 N14 180.0(3) 9_556 3 ?
N14 Fe1 N14 89.4(3) 5 7_556 ?
N14 Fe1 N14 90.6(3) 9_556 7_556 ?
N14 Fe1 N14 90.6(3) 11_556 7_556 ?
N14 Fe1 N14 90.6(3) 3 . ?
N14 Fe1 N14 89.4(3) 11_556 . ?
N14 Fe1 N14 89.4(3) 9_556 5 ?
N14 Fe1 N14 90.6(3) 9_556 11_556 ?
N14 Fe1 N14 90.6(3) 3 5 ?
N14 Fe1 N14 89.4(3) 9_556 . ?
N14 Fe1 N14 180.0(3) 11_556 5 ?
N14 Fe1 N14 89.4(3) 3 11_556 ?
N14 Fe1 N14 90.6(3) 5 . ?
N14 Fe1 N14 89.4(3) 3 7_556 ?
N14 Fe1 N14 180.0 7_556 . ?
C8 N14 Fe1 130.9(7) . . ?
C8 N14 N13 104.7(8) . . ?
N13 N14 Fe1 124.2(6) . . ?
N7 N3 C3 120.4(9) . . ?
C8 N3 N7 109.7(9) . . ?
C8 N3 C3 129.8(10) . . ?
N13 N7 N3 106.2(8) . . ?
N14 C8 H8 125.7 . . ?
N3 C8 N14 108.6(9) . . ?
N3 C8 H8 125.7 . . ?
N7 N13 N14 110.7(8) . . ?
N3 C3 H3A 109.4 . . ?
N3 C3 H3B 109.4 . . ?
N3 C3 C4 111.2(8) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C1 C4 C3 120.4(7) . . ?
C1 C4 C2 116.9(8) . . ?
C2 C4 C3 122.7(7) . . ?
C4 C1 H1 119.2 . . ?
C1 C1 C4 121.5(4) 10_557 . ?
C1 C1 H1 119.2 10_557 . ?
C4 C2 C2 121.5(4) . 10_557 ?
C4 C2 H2 119.2 . . ?
C2 C2 H2 119.2 10_557 . ?
F1 B0AA F1 118.6(3) 3_445 . ?
F1 B0AA F1 118.6(3) 5_545 3_445 ?
F1 B0AA F1 118.6(3) 5_545 . ?
F1 B0AA F2 96.7(8) 5_545 . ?
F1 B0AA F2 96.7(8) . . ?
F1 B0AA F2 96.7(8) 3_445 . ?
F2A B0AA F2A 119.6(3) 5_545 . ?
F2A B0AA F2A 119.6(3) 5_545 3_445 ?
F2A B0AA F2A 119.6(3) 3_445 . ?
F2A B0AA F1A 93.4(14) 5_545 . ?
F2A B0AA F1A 93.4(14) 3_445 . ?
F2A B0AA F1A 93.4(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
Fe1 N14 C8 N3 -173.9(6) . . . . ?
Fe1 N14 N13 N7 175.9(7) . . . . ?
N3 N7 N13 N14 -1.6(14) . . . . ?
N3 C3 C4 C1 -116.3(11) . . . . ?
N3 C3 C4 C2 65.1(14) . . . . ?
N7 N3 C8 N14 -2.7(12) . . . . ?
N7 N3 C3 C4 55.6(13) . . . . ?
C8 N14 N13 N7 -0.1(12) . . . . ?
C8 N3 N7 N13 2.7(13) . . . . ?
C8 N3 C3 C4 -130.1(11) . . . . ?
N13 N14 C8 N3 1.7(11) . . . . ?
C3 N3 N7 N13 178.0(9) . . . . ?
C3 N3 C8 N14 -177.5(9) . . . . ?
C3 C4 C1 C1 -179.2(6) . . . 10_557 ?
C3 C4 C2 C2 179.1(7) . . . 10_557 ?
C1 C4 C2 C2 0.6(13) . . . 10_557 ?
C2 C4 C1 C1 -0.6(13) . . . 10_557 ?

_shelx_res_file                  
;
TITL sx317 in P63/m #176
REM reset to P63/m #176
CELL 0.71073 10.4852 10.4852 23.3082 90 90 120
ZERR 2 0.001 0.001 0.0028 0 0 0
LATT 1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SFAC C H B F Fe N
UNIT 60 60 4 16 2 48
EQIV $1 +X,+Y,1.5-Z
DFIX 2 F2A F1A
SADI 0.002 C1 C1_$1 C4_$1 C1_$1 C4_$1 C2_$1 C2 C2_$1 C4 C2 C4 C1
SADI 0.002 F1 B0AA F2 B0AA
SADI 0.002 F2A B0AA F1 B0AA F1A B0AA F2 B0AA
SIMU 0.002 0.004 2 F1 F2 F2A F1A
RIGU C2 C4 C1 C3
RIGU N14 C8 N3 N7 N13
RIGU 0.02 0.02 F2A F1 F1A B0AA F2

L.S. 15
PLAN  20
TEMP -33
BOND
MORE -1
BOND $H
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\sx317twin.hkl">
REM </olex2.extras>

WGHT    0.110400
BASF   0.37975
FVAR       9.89306   0.86507
FE1   5    0.000000    0.000000    0.500000    10.16667    0.03821    0.03821 =
         0.03373    0.00000    0.00000    0.01910
N14   6   -0.142333   -0.185797    0.552663    11.00000    0.04309    0.03675 =
         0.03970    0.00076   -0.00324    0.01780
N3    6   -0.323015   -0.351265    0.601723    11.00000    0.04402    0.04764 =
         0.04099    0.01075    0.00012    0.01906
N7    6   -0.203443   -0.357808    0.617150    11.00000    0.05428    0.08150 =
         0.08769    0.04937    0.00774    0.03265
C8    1   -0.288051   -0.251470    0.562106    11.00000    0.04377    0.04660 =
         0.04038    0.01123    0.00103    0.02171
AFIX  43
H8    2   -0.353797   -0.229166    0.543283    11.00000   -1.20000
AFIX   0
N13   6   -0.094773   -0.256293    0.588055    11.00000    0.04744    0.07151 =
         0.07662    0.03708    0.00580    0.02797
C3    1   -0.468995   -0.456742    0.625796    11.00000    0.04484    0.06006 =
         0.04144    0.00825    0.00206    0.01090
AFIX  23
H3A   2   -0.498000   -0.556409    0.612667    11.00000   -1.20000
H3B   2   -0.542336   -0.432300    0.611809    11.00000   -1.20000
AFIX   0
C4    1   -0.466343   -0.452950    0.690049    11.00000    0.03511    0.05570 =
         0.03393    0.00272   -0.00058    0.01550
C1    1   -0.491251   -0.574307    0.720700    11.00000    0.09433    0.05464 =
         0.03767   -0.00103    0.00172    0.02817
AFIX  43
H1    2   -0.508804   -0.659827    0.701007    11.00000   -1.20000
AFIX   0
C2    1   -0.442699   -0.331974    0.720696    11.00000    0.08464    0.07329 =
         0.05126   -0.00370   -0.00991    0.04213
AFIX  43
H2    2   -0.426045   -0.246758    0.700998    11.00000   -1.20000
AFIX   0

PART 1
F1    4   -0.341073   -0.540751    0.499599    21.00000    0.11991    0.11078 =
         0.14604   -0.00487    0.00265    0.07693
F2    4   -0.333333   -0.666667    0.433774    20.33333    0.12832    0.12832 =
         0.14695    0.00000    0.00000    0.06416
PART 0
B0AA  3   -0.333333   -0.666667    0.492685    10.33333    0.10430    0.10430 =
         0.05964    0.00000    0.00000    0.05215
PART 2
F2A   4   -0.332030   -0.535338    0.489148   -20.33333    0.12344    0.12016 =
         0.14638   -0.00176    0.00097    0.06778
F1A   4   -0.333333   -0.666667    0.551586   -21.00000    0.12244    0.12244 =
         0.14632    0.00000    0.00000    0.06122
HKLF 5

REM  sx317 in P63/m #176
REM R1 =  0.1085 for     608 Fo > 4sig(Fo)  and  0.2252 for all    1400 data
REM    113 parameters refined using    112 restraints

END

WGHT      0.1540      0.0000

REM Highest difference peak  1.200,  deepest hole -1.000,  1-sigma level  0.129
Q1    1   0.0000  0.0000  0.7288  10.33333  0.05    1.20
Q2    1  -0.0866  0.0275  0.7500  10.50000  0.05    0.57
Q3    1  -0.2615 -0.5386  0.5270  11.00000  0.05    0.46
Q4    1  -0.4477 -0.6311  0.5031  11.00000  0.05    0.45
Q5    1  -0.1537 -0.0966  0.7500  10.50000  0.05    0.40
Q6    1  -0.5696 -0.5981  0.5543  11.00000  0.05    0.38
Q7    1  -0.4678 -0.5621  0.5023  11.00000  0.05    0.38
Q8    1  -0.6548 -0.6657  0.5998  11.00000  0.05    0.35
Q9    1   0.0419 -0.1563  0.6157  11.00000  0.05    0.34
Q10   1  -0.5772 -0.4624  0.7197  11.00000  0.05    0.31
Q11   1  -0.3469 -0.4324  0.4716  11.00000  0.05    0.30
Q12   1  -0.4250 -0.3888  0.5019  11.00000  0.05    0.29
Q13   1  -0.0009 -0.2648  0.5546  11.00000  0.05    0.29
Q14   1  -0.3280 -0.2334  0.5678  11.00000  0.05    0.29
Q15   1  -0.6379 -0.7813  0.7500  10.50000  0.05    0.28
Q16   1  -0.2040 -0.4211  0.5308  11.00000  0.05    0.28
Q17   1  -0.1194 -0.0613  0.6866  11.00000  0.05    0.28
Q18   1  -0.2749 -0.2560  0.7500  10.50000  0.05    0.28
Q19   1  -0.6035 -0.5219  0.5830  11.00000  0.05    0.28
Q20   1  -0.4012 -0.4989  0.5726  11.00000  0.05    0.27
;
_shelx_res_checksum              61813
_olex2_date_sample_data_collection 2012-12-04
_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 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.877
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.620(8)
2 0.380(8)

_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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_CCP-2_LS
_database_code_depnum_ccdc_archive 'CCDC 1439097'
_audit_update_record             
;
2016-10-13 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;
_audit_creation_date             2016-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H60 Fe2 N48), 4.63(B0.43 F1.73)'
_chemical_formula_sum            'C30 H30 B2 F8 Fe N24'
_chemical_formula_weight         956.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'

_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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   10.3690(5)
_cell_length_b                   10.3690(5)
_cell_length_c                   22.9628(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2138.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    877
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.9582
_cell_measurement_theta_min      3.4904
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.978
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            1300
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         3.497
_diffrn_reflns_v_R_equivalents   ?
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                981
_reflns_number_total             1300
_reflns_special_details          
;
 _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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.320
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1300
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1090
_refine_ls_restrained_S_all      1.074
_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)+(0.1380P)²+19.7224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2739
_refine_ls_wR_factor_ref         0.2978
_refine_special_details          'Refined as a 2-component twin., Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.631(8) 0.369(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups
3. Restrained distances
 B1-F1
 1.38 with sigma of 0.01
 B1-F2
 1.38 with sigma of 0.01
 B1'-F1'
 1.38 with sigma of 0.01
 B1'-F2'
 1.38 with sigma of 0.01
4. Rigid body (RIGU) restrains
 B1, F1, F2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F2', B1', F1'
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F2')=1-FVAR(1)
 Sof(B1')=Sof(F1')=0.33333*(1-FVAR(2))
 Sof(B1)=Sof(F1)=0.33333*FVAR(2)
 Sof(F2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9)
6.c Fitted pentagon refined as free rotating group:
 N1(C2,N3,N4,N5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -1.0000 0.0000 0.5000 0.0145(7) Uani 1 6 d S T P . .
B1 B -0.3333 0.3333 0.5157(10) 0.031(8) Uani 0.43(2) 3 d DS TU P A 1
F1 F -0.3333 0.3333 0.5760(9) 0.034(6) Uani 0.43(2) 3 d DS TU P A 1
F2 F -0.340(6) 0.203(3) 0.4971(12) 0.047(9) Uani 0.43(2) 1 d D U . A 1
B1' B -0.6667 -0.3333 0.5097(7) 0.029(6) Uani 0.57(2) 3 d DS TU P A 2
F1' F -0.6667 -0.3333 0.5699(7) 0.042(5) Uani 0.57(2) 3 d DS TU P A 2
F2' F -0.655(3) -0.2011(18) 0.4901(8) 0.033(5) Uani 0.57(2) 1 d D U . A 2
N1 N -0.8714(5) -0.0409(6) 0.5480(2) 0.0175(17) Uani 1 1 d . . . . .
C2 C -0.7159(5) 0.0481(5) 0.5580(2) 0.023(2) Uani 1 1 d G . . . .
H2 H -0.6508 0.1407 0.5399 0.027 Uiso 1 1 calc R . . . .
N3 N -0.6748(5) -0.0258(7) 0.5998(2) 0.029(2) Uani 1 1 d G . . . .
N4 N -0.8049(6) -0.1603(6) 0.6156(2) 0.039(2) Uani 1 1 d G . . . .
N5 N -0.9264(5) -0.1697(5) 0.5836(3) 0.036(2) Uani 1 1 d G . . . .
C6 C -0.5405(12) 0.0087(16) 0.6231(4) 0.032(2) Uani 1 1 d . . . . .
H6A H -0.4638 0.1072 0.6082 0.048 Uiso 1 1 calc R . . . .
H6B H -0.5137 -0.0657 0.6099 0.048 Uiso 1 1 calc R . . . .
C7 C -0.5386(10) 0.0130(12) 0.6895(3) 0.0220(19) Uani 1 1 d . . . . .
C8 C -0.5611(13) 0.1156(12) 0.7197(4) 0.032(2) Uani 1 1 d . . . . .
H8 H -0.5766 0.1861 0.6990 0.038 Uiso 1 1 calc R . . . .
C9 C -0.5153(11) -0.0867(12) 0.7201(4) 0.028(2) Uani 1 1 d . . . . .
H9 H -0.4989 -0.1569 0.6997 0.034 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0151(9) 0.0151(9) 0.0132(13) 0.000 0.000 0.0076(5)
B1 0.024(11) 0.024(11) 0.044(11) 0.000 0.000 0.012(5)
F1 0.029(8) 0.029(8) 0.045(11) 0.000 0.000 0.014(4)
F2 0.07(2) 0.029(10) 0.051(12) -0.001(5) 0.005(8) 0.027(10)
B1' 0.027(8) 0.027(8) 0.033(8) 0.000 0.000 0.014(4)
F1' 0.047(8) 0.047(8) 0.033(7) 0.000 0.000 0.023(4)
F2' 0.035(11) 0.030(8) 0.036(7) 0.001(4) 0.002(6) 0.017(6)
N1 0.022(4) 0.012(4) 0.016(3) 0.005(3) 0.007(3) 0.007(3)
C2 0.027(5) 0.038(6) 0.008(4) -0.002(4) -0.006(4) 0.020(5)
N3 0.022(4) 0.039(6) 0.021(4) 0.003(4) 0.000(3) 0.013(4)
N4 0.039(6) 0.024(5) 0.050(5) 0.019(4) 0.002(5) 0.013(5)
N5 0.035(5) 0.035(5) 0.040(5) 0.016(4) -0.009(4) 0.018(4)
C6 0.030(6) 0.050(7) 0.021(4) 0.006(5) 0.002(4) 0.023(6)
C7 0.017(5) 0.029(5) 0.020(4) -0.002(4) -0.004(4) 0.011(4)
C8 0.038(6) 0.033(6) 0.028(5) 0.002(5) -0.004(5) 0.020(5)
C9 0.038(6) 0.040(6) 0.021(4) 0.004(4) 0.004(4) 0.031(5)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.933(4) 8_446 ?
Fe1 N1 1.933(4) . ?
Fe1 N1 1.933(4) 2_465 ?
Fe1 N1 1.933(4) 3_345 ?
Fe1 N1 1.933(4) 7_356 ?
Fe1 N1 1.933(4) 9_566 ?
B1 F1 1.384(10) . ?
B1 F2 1.387(10) . ?
B1 F2 1.387(10) 2_565 ?
B1 F2 1.387(10) 3_455 ?
B1' F1' 1.381(10) . ?
B1' F2' 1.392(9) . ?
B1' F2' 1.392(9) 2_455 ?
B1' F2' 1.392(9) 3_445 ?
N1 C2 1.4200 . ?
N1 N5 1.4200 . ?
C2 H2 0.9500 . ?
C2 N3 1.4200 . ?
N3 N4 1.4200 . ?
N3 C6 1.362(10) . ?
N4 N5 1.4200 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.526(12) . ?
C7 C8 1.384(14) . ?
C7 C9 1.367(14) . ?
C8 C8 1.392(19) 10_557 ?
C8 H8 0.9500 . ?
C9 C9 1.373(17) 10_557 ?
C9 H9 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 180.0(2) 8_446 2_465 ?
N1 Fe1 N1 180.0 9_566 3_345 ?
N1 Fe1 N1 89.3(2) 8_446 3_345 ?
N1 Fe1 N1 89.3(2) 7_356 3_345 ?
N1 Fe1 N1 90.7(2) 2_465 . ?
N1 Fe1 N1 89.3(2) 9_566 . ?
N1 Fe1 N1 90.7(2) 8_446 9_566 ?
N1 Fe1 N1 90.7(2) 8_446 7_356 ?
N1 Fe1 N1 89.3(2) 2_465 9_566 ?
N1 Fe1 N1 89.3(2) 8_446 . ?
N1 Fe1 N1 90.7(2) 7_356 9_566 ?
N1 Fe1 N1 89.3(2) 2_465 7_356 ?
N1 Fe1 N1 180.0(3) 7_356 . ?
N1 Fe1 N1 90.7(2) 2_465 3_345 ?
N1 Fe1 N1 90.7(2) 3_345 . ?
F1 B1 F2 107.9(14) . . ?
F1 B1 F2 107.9(14) . 3_455 ?
F1 B1 F2 107.9(14) . 2_565 ?
F2 B1 F2 111.0(13) . 3_455 ?
F2 B1 F2 111.0(13) . 2_565 ?
F2 B1 F2 111.0(13) 2_565 3_455 ?
F1' B1' F2' 108.9(9) . . ?
F1' B1' F2' 108.9(9) . 3_445 ?
F1' B1' F2' 108.9(9) . 2_455 ?
F2' B1' F2' 110.0(9) . 3_445 ?
F2' B1' F2' 110.0(9) . 2_455 ?
F2' B1' F2' 110.0(9) 2_455 3_445 ?
C2 N1 Fe1 129.3(3) . . ?
C2 N1 N5 108.0 . . ?
N5 N1 Fe1 122.5(3) . . ?
N1 C2 H2 126.0 . . ?
N3 C2 N1 108.0 . . ?
N3 C2 H2 126.0 . . ?
C2 N3 N4 108.0 . . ?
C6 N3 C2 131.8(7) . . ?
C6 N3 N4 120.1(7) . . ?
N5 N4 N3 108.0 . . ?
N4 N5 N1 108.0 . . ?
N3 C6 H6A 108.9 . . ?
N3 C6 H6B 108.9 . . ?
N3 C6 C7 113.4(8) . . ?
H6A C6 H6B 107.7 . . ?
C7 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
C8 C7 C6 121.2(9) . . ?
C9 C7 C6 119.8(10) . . ?
C9 C7 C8 119.0(8) . . ?
C7 C8 C8 120.0(5) . 10_557 ?
C7 C8 H8 120.0 . . ?
C8 C8 H8 120.0 10_557 . ?
C7 C9 C9 120.9(5) . 10_557 ?
C7 C9 H9 119.5 . . ?
C9 C9 H9 119.5 10_557 . ?

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
Fe1 N1 C2 N3 175.9(5) . . . . ?
Fe1 N1 N5 N4 -176.2(4) . . . . ?
N1 C2 N3 N4 0.0 . . . . ?
N1 C2 N3 C6 177.7(9) . . . . ?
C2 N1 N5 N4 0.0 . . . . ?
C2 N3 N4 N5 0.0 . . . . ?
C2 N3 C6 C7 125.7(9) . . . . ?
N3 N4 N5 N1 0.0 . . . . ?
N3 C6 C7 C8 -63.5(15) . . . . ?
N3 C6 C7 C9 116.0(11) . . . . ?
N4 N3 C6 C7 -56.8(13) . . . . ?
N5 N1 C2 N3 0.0 . . . . ?
C6 N3 N4 N5 -178.0(8) . . . . ?
C6 C7 C8 C8 179.0(7) . . . 10_557 ?
C6 C7 C9 C9 -179.0(6) . . . 10_557 ?
C8 C7 C9 C9 0.5(12) . . . 10_557 ?
C9 C7 C8 C8 -0.5(12) . . . 10_557 ?

_shelx_res_file                  
;
TITL sx318bb in P6(3)/m
CELL 0.71073 10.369 10.369 22.9628 90 90 120
ZERR 2 0.0005 0.0005 0.0015 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SFAC C H B F Fe N
UNIT 60 60 4 16 2 48
DFIX 1.38 0.01 B1 F1
DFIX 1.38 0.01 B1 F2
DFIX 1.38 0.01 B1' F1'
DFIX 1.38 0.01 B1' F2'
RIGU 0.002 0.002 B1 F1 F2
RIGU 0.002 0.002 F2' B1' F1'

L.S. 10
PLAN  20
SIZE 0.05 0.05 0.02
TEMP -153
BOND
MORE -1
BOND $H
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\sx318bbtwinb.hkl">
REM </olex2.extras>

WGHT    0.138000   19.722403
SWAT    0.000044  231.1549
BASF   0.36852
FVAR       9.36295   0.43195
FE1   5   -1.000000    0.000000    0.500000    10.16667    0.01512    0.01512 =
         0.01316    0.00000    0.00000    0.00756
PART 1
B1    3   -0.333333    0.333333    0.515661    20.33333    0.02422    0.02422 =
         0.04419    0.00000    0.00000    0.01211
F1    4   -0.333333    0.333333    0.575952    20.33333    0.02877    0.02877 =
         0.04487    0.00000    0.00000    0.01439
F2    4   -0.340261    0.202728    0.497070    21.00000    0.06515    0.02891 =
         0.05098   -0.00067    0.00519    0.02690

PART 0
PART 2
B1'   3   -0.666667   -0.333333    0.509750   -20.33333    0.02737    0.02737 =
         0.03347    0.00000    0.00000    0.01369
F1'   4   -0.666667   -0.333333    0.569905   -20.33333    0.04681    0.04681 =
         0.03333    0.00000    0.00000    0.02341
F2'   4   -0.655365   -0.201085    0.490088   -21.00000    0.03491    0.02970 =
         0.03619    0.00072    0.00206    0.01677

PART 0
AFIX  56
N1    6   -0.871415   -0.040887    0.547969    11.00000    0.02227    0.01208 =
         0.01632    0.00505    0.00654    0.00716
C2    1   -0.715908    0.048053    0.557990    11.00000    0.02728    0.03761 =
         0.00812   -0.00209   -0.00649    0.02020
AFIX  43
H2    2   -0.650810    0.140676    0.539889    11.00000   -1.20000
AFIX  55
N3    6   -0.674790   -0.025763    0.599816    11.00000    0.02204    0.03917 =
         0.02098    0.00287   -0.00016    0.01276
N4    6   -0.804884   -0.160323    0.615645    11.00000    0.03898    0.02421 =
         0.05015    0.01904    0.00170    0.01345
N5    6   -0.926406   -0.169670    0.583602    11.00000    0.03498    0.03470 =
         0.03973    0.01598   -0.00908    0.01842
AFIX   0
C6    1   -0.540505    0.008745    0.623090    11.00000    0.02958    0.05000 =
         0.02068    0.00623    0.00189    0.02282
AFIX  23
H6A   2   -0.463810    0.107207    0.608179    11.00000   -1.50000
H6B   2   -0.513704   -0.065732    0.609890    11.00000   -1.50000
AFIX   0
C7    1   -0.538575    0.012989    0.689507    11.00000    0.01693    0.02852 =
         0.02008   -0.00163   -0.00366    0.01090
C8    1   -0.561124    0.115574    0.719685    11.00000    0.03846    0.03275 =
         0.02764    0.00158   -0.00366    0.02037
AFIX  43
H8    2   -0.576617    0.186050    0.699015    11.00000   -1.20000
AFIX   0
C9    1   -0.515317   -0.086665    0.720100    11.00000    0.03797    0.04018 =
         0.02135    0.00365    0.00355    0.03078
AFIX  43
H9    2   -0.498925   -0.156906    0.699703    11.00000   -1.20000
AFIX   0
HKLF 5

REM  sx318bb in P6(3)/m
REM R1 =  0.1090 for     981 Fo > 4sig(Fo)  and  0.1389 for all    1300 data
REM    109 parameters refined using     22 restraints

END

WGHT      0.1449     18.8697

REM Highest difference peak  2.320,  deepest hole -1.012,  1-sigma level  0.168
Q1    1  -1.0000  0.0000  0.7227  10.33333  0.05    2.32
Q2    1  -1.0000  0.0000  0.6806  10.33333  0.05    0.76
Q3    1  -0.3333  0.3333  0.7080  10.33333  0.05    0.51
Q4    1  -0.3903  0.0301  0.7500  10.50000  0.05    0.47
Q5    1  -0.6667 -0.3333  0.7500  10.16667  0.05    0.41
Q6    1  -0.9069 -0.2542  0.5970  11.00000  0.05    0.40
Q7    1  -0.6618  0.1784  0.6101  11.00000  0.05    0.37
Q8    1  -0.4302 -0.0853  0.6929  11.00000  0.05    0.37
Q9    1  -0.6115 -0.0865  0.7010  11.00000  0.05    0.37
Q10   1  -0.8164  0.0217  0.7500  10.50000  0.05    0.36
Q11   1  -0.4994 -0.0016  0.6006  11.00000  0.05    0.36
Q12   1  -0.4554  0.0077  0.6996  11.00000  0.05    0.35
Q13   1  -0.6418 -0.2032  0.7047  11.00000  0.05    0.34
Q14   1  -0.5514  0.0051  0.6639  11.00000  0.05    0.34
Q15   1  -0.5008 -0.2993  0.6623  11.00000  0.05    0.34
Q16   1  -0.3659 -0.1226  0.7500  10.50000  0.05    0.34
Q17   1  -0.4084  0.3368  0.6761  11.00000  0.05    0.34
Q18   1  -0.5481 -0.1507  0.7500  10.50000  0.05    0.33
Q19   1  -0.6694 -0.1459  0.7500  10.50000  0.05    0.33
Q20   1  -0.7845 -0.0200  0.5004  11.00000  0.05    0.33
;
_shelx_res_checksum              6907
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.631(8)
2 0.369(8)

_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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_ccp1_co2
_database_code_depnum_ccdc_archive 'CCDC 1473649'
_audit_update_record             
;
2016-04-12 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H30 Fe N24, 1.122(CO2), 2(Cl O4)'
_chemical_formula_structural     'Fe (C10 H10 N8)3, 2(ClO4) 1.122(CO2)'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C31.12 H30 Cl2 Fe N24 O10.24'
_chemical_formula_weight         1053.4
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Hexagonal
_space_group_name_H-M_alt        P63/m
_space_group_name_Hall           -P_6c
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'

_cell_length_a                   10.55931(6)
_cell_length_b                   10.55931(6)
_cell_length_c                   23.6672(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2285.33(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4981(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1053.4



# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              10
# perpendicular to equatorial plane
_pd_spec_size_equat              1
# parallel to scattering vector  in transmission
_pd_spec_size_thick              ?
# parallel to scattering vector  in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                '1 mm borosilicate capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'visual estimate, prisms'
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.
_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; Diamond Light Source
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_radiation_wavelength     0.799933
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  'BEamline BL04, ALBA'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 ?
_diffrn_detector_type            '40 degrees Mythen'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        6850
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.003

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_number            628

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_data_reduction        'Topas (Coelho, 2003)'
_computing_structure_solution    'Topas (Coelho, 2003)'
_computing_structure_refinement  'Topas (Coelho, 2003)'
_computing_publication_material  
'enCifer (Cambridge Crystallographic Data Centre, 2004)'

#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; 
The structure solution was obtained by global optimisation using the
DASH structure solution program.  The internal coordinate 
description of the molecule was constructed from standard bond
lengths, bond angles and bond torsions where appropriate.
 The structure was refined against data in the range 
3.0 to 40.0° 2θ (628 reflections).
;

# The next three items are given as text
_pd_proc_ls_profile_function     
;   
Fundamental parameters with axial divergence correction
;
_pd_proc_ls_background_function  
;
Chebyshev polynomial
;
_pd_proc_ls_pref_orient_corr     
; 
A spherical harmonics-based preferred orientation correction 
was applied with Topas during the Rietveld refinement.
;

_pd_proc_ls_prof_R_wp_factor     0.02144
_pd_proc_ls_prof_R_wp_dash_factor 0.09705
_pd_proc_ls_prof_wR_expected     0.00982

_refine_special_details          'powder data'

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     62
_refine_ls_number_restraints     56
_refine_ls_number_constraints    1

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   2.183

_refine_ls_R_I_factor            ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?



# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id       ccp_1_co2_6bar_fsum.xye

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe 0 1 1 0.5 1 3.478(96)
O1 O 0 0.802 0.4505 0.4954 1 10.65(23)
Cl1 Cl 0 0.6666667 0.3333333 0.5075 0.5930(54) 5.80(47)
O2 O 0 0.6666667 0.3333333 0.5655 0.5930(54) 5.80(47)
Cl1b Cl 0 0.6666667 0.3333333 0.4871 0.4070(54) 5.04(71)
O2b O 0 0.6666667 0.3333333 0.4284 0.4070(54) 5.04(71)
N1 N 0 0.95445 0.81195 0.55218 1 5.455(98)
C2 C 0 1.0339 0.7515 0.562 1 5.455(98)
H2 H 0 1.13437 0.777224 0.539852 1 6.55(12)
N3 N 0 0.9733 0.6528 0.6027 1 5.455(98)
N4 N 0 0.8471 0.6465 0.6184 1 5.455(98)
N5 N 0 0.8391 0.7484 0.5887 1 5.455(98)
C6 C 0 1.0125 0.548 0.6262 1 5.455(98)
H6A H 0 1.11982 0.57411 0.61049 1 6.55(12)
H6B H 0 0.933757 0.438291 0.611823 1 6.55(12)
C7 C 0 1.0152 0.5501 0.6909 1 5.455(98)
C8 C 0 1.1143 0.6718 0.7201 1 5.455(98)
H8 H 0 1.19327 0.768865 0.69716 1 6.55(12)
C9 C 0 0.9163 0.4277 0.7208 1 5.455(98)
H9 H 0 0.837515 0.330113 0.698076 1 6.55(12)
O1S O 0 0.123155 -0.02252587 0.1889301 0.1872(12) 8
C1S C 0 0.07618873 0.04246368 0.2116206 0.1872(12) 8
O2S O 0 0.02922247 0.1074532 0.234311 0.1872(12) 8




# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag


# C8     C8        1.4153(1)       .     10_556       no                                                           
# C9     C9        1.3822(1)       .     10_556       no




# Cl1    O1         1.3736     .     3_655      no
# Cl1    O1         1.3736      .     5_665      no
Fe1 N1 2.1781(1) . . no
N1 N5 1.3651(1) . . no
N1 C2 1.3041(1) . . no
N3 N4 1.3526(1) . . no
N3 C2 1.3254(1) . . no
N3 C6 1.4708(1) . . no
N4 N5 1.3228(1)) . . no
C6 C7 1.5315(1) . . no
C7 C8 1.3709(1) . . no
C7 C9 1.3828(1) . . no
C2 H2 1.09 . . no
C6 H6A 1.09 . . no
C6 H6B 1.09 . . no
C8 H8 1.09 . . no
C9 H9 1.09 . . no
O1S C1S 1.160 . . no
O2S C1S 1.160 . . no
Cl1 O1 1.3736(1) . . no
Cl1 O2 1.3727(1) . . no
Cl1B O1 1.3577(1) . . no
Cl1B O2B 1.3893(1) . . no
# Cl1B   O1           1.3577     .     3_655      no                                    
# Cl1B   O1          1.3577     .     5_665      no







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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag







N1 Fe1 N1 91.02 . . 3_555 no
N1 Fe1 N1 180.00 . . 7_555 no
N1 Fe1 N1 88.98 . . 9_555 no
Fe1 N1 N5 122.90 . . . no
Fe1 N1 C2 130.12 . . . no
N5 N1 C2 106.31 . . . no
N4 N3 C2 108.35 . . . no
N4 N3 C6 120.00 . . . no
C2 N3 C6 131.27 . . . no
N3 N4 N5 106.02 . . . no
N1 N5 N4 109.40 . . . no
N1 C2 N3 109.79 . . . no
N3 C6 C7 112.17 . . . no
C6 C7 C8 121.17 . . . no
C6 C7 C9 119.88 . . . no
C8 C7 C9 118.95 . . . no
C7 C8 C8 120.27 . . 10_556 no
C7 C9 C9 120.78 . . 10_556 no
N1 C2 H2 125 . . . no
N3 C2 H2 125 . . . no
N3 C6 H6A 109 . . . no
N3 C6 H6B 109 . . . no
C7 C6 H6A 109 . . . no
C7 C6 H6B 109 . . . no
H6A C6 H6B 108 . . . no
C7 C8 H8 120 . . . no
H8 C8 C8 120 . . 10_555 no
C7 C9 H9 120 . . . no
H9 C9 C9 120 . . 10_555 no
O1S C1S O2S 179.98 . . . no
O1 Cl1 O2 102.03 . . . no
O1 Cl1 O1 115.77 . . 3_655 no
O1 Cl1B O2B 98.32 . . . no
O1 Cl1B O1 117.94 . . 3_655 no



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






N1 Fe1 N1 N5 107.47 3_555 . . . no
N1 Fe1 N1 C2 -61.76 3_555 . . . no
N1 Fe1 N1 N5 16.43 5_555 . . . no
N1 Fe1 N1 C2 -152.80 5_555 . . . no
N1 Fe1 N1 N5 -72.53 9_555 . . . no
N1 Fe1 N1 C2 118.24 9_555 . . . no
N1 Fe1 N1 N5 -163.57 11_555 . . . no
N1 Fe1 N1 C2 27.20 11_555 . . . no
Fe1 N1 N5 N4 -173.98 . . . . no
C2 N1 N5 N4 -2.54 . . . . no
Fe1 N1 C2 N3 170.89 . . . . no
N5 N1 C2 N3 0.30 . . . . no
C2 N3 N4 N5 -3.48 . . . . no
C6 N3 N4 N5 -177.18 . . . . no
N4 N3 C2 N1 1.99 . . . . no
C6 N3 C2 N1 174.72 . . . . no
N4 N3 C6 C7 -55.68 . . . . no
C2 N3 C6 C7 132.27 . . . . no
N3 N4 N5 N1 3.69 . . . . no
N3 C6 C7 C8 -64.60 . . . . no
N3 C6 C7 C9 115.34 . . . . no
C6 C7 C8 C8 179.57 . . . 10_555 no
C9 C7 C8 C8 -0.36 . . . 10_555 no
C6 C7 C9 C9 -179.57 . . . 10_555 no
C8 C7 C9 C9 0.36 . . . 10_555 no
Fe1 N1 C2 H2 -10 . . . . no
N5 N1 C2 H2 180 . . . . no
N4 N3 C2 H2 -177 . . . . no
C6 N3 C2 H2 -5 . . . . no
N4 N3 C6 H6A -177 . . . . no
N4 N3 C6 H6B 65 . . . . no
C2 N3 C6 H6A 11 . . . . no
C2 N3 C6 H6B -107 . . . . no
H6A C6 C7 C8 57 . . . . no
H6A C6 C7 C9 -123 . . . . no
H6B C6 C7 C8 174 . . . . no
H6B C6 C7 C9 -6 . . . . no
C6 C7 C8 H8 0 . . . . no
C9 C7 C8 H8 180 . . . . no
C6 C7 C9 H9 0 . . . . no
C8 C7 C9 H9 -180 . . . . no
C7 C8 C8 H8 -180 . . 10_555 10_555 no
C7 C9 C9 H9 -180 . . 10_555 10_555 no





















_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_ccp1_C2H4
_database_code_depnum_ccdc_archive 'CCDC 1473650'
_audit_update_record             
;
2016-04-12 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H30 Fe N24, 2(Cl O4), 0.816(C2 H4)'
_chemical_formula_structural     'Fe (C10 H10 N8)3, 2(ClO4) 0.816(C2H4)'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C31.63 H33.26 Cl2 Fe N24 O8'
_chemical_formula_weight         1004.42
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Hexagonal
_space_group_name_H-M_alt        P63/m
_space_group_name_Hall           -P_6c
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'

_cell_length_a                   10.52034(6)
_cell_length_b                   10.52034(6)
_cell_length_c                   23.5917(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2261.25(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4752(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1030.1



# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              10
# perpendicular to equatorial plane
_pd_spec_size_equat              1
# parallel to scattering vector  in transmission
_pd_spec_size_thick              ?
# parallel to scattering vector  in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                '1 mm borosilicate capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'visual estimate, prisms'
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.
_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; Diamond Light Source
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_radiation_wavelength     0.799933
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  'BEamline BL04, ALBA'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 ?
_diffrn_detector_type            '40 degrees Mythen'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        6850
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.003

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_number            628

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_data_reduction        'Topas (Coelho, 2003)'
_computing_structure_solution    'Topas (Coelho, 2003)'
_computing_structure_refinement  'Topas (Coelho, 2003)'
_computing_publication_material  
'enCifer (Cambridge Crystallographic Data Centre, 2004)'

#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; 
The structure solution was obtained by global optimisation using the
DASH structure solution program.  The internal coordinate 
description of the molecule was constructed from standard bond
lengths, bond angles and bond torsions where appropriate.
 The structure was refined against data in the range 
2.0 to 40.0° 2θ (628 reflections).
;

# The next three items are given as text
_pd_proc_ls_profile_function     
;   
Fundamental parameters with axial divergence correction
;
_pd_proc_ls_background_function  
;
Chebyshev polynomial
;
_pd_proc_ls_pref_orient_corr     
; 
A spherical harmonics-based preferred orientation correction 
was applied with Topas during the Rietveld refinement.
;

_pd_proc_ls_prof_R_wp_factor     0.01615
_pd_proc_ls_prof_R_wp_dash_factor 0.10951
_pd_proc_ls_prof_wR_expected     0.00841

_refine_special_details          'powder data'

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     61
_refine_ls_number_restraints     56
_refine_ls_number_constraints    1

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.919

_refine_ls_R_I_factor            ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?



# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id       ccp_1_C2H4_6bar_fsum.xye

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe 0 1 1 0.5 1 3.65836
O1 O 0 0.802 0.4505 0.4954 1 10.09675
Cl1 Cl 0 0.6666667 0.3333333 0.5075 0.61813 10.70945
O2 O 0 0.6666667 0.3333333 0.5655 0.61813 10.70945
Cl1b Cl 0 0.6666667 0.3333333 0.4871 0.38187 0.15756
O2b O 0 0.6666667 0.3333333 0.4284 0.38187 0.15756
N1 N 0 0.95445 0.81195 0.55218 1 6.1921
C2 C 0 1.0339 0.7515 0.562 1 6.1921
H2 H 0 1.13473 0.777316 0.539773 1 -1.2
N3 N 0 0.9733 0.6528 0.6027 1 6.1921
N4 N 0 0.8471 0.6465 0.6184 1 6.1921
N5 N 0 0.8391 0.7484 0.5887 1 6.1921
C6 C 0 1.0125 0.548 0.6262 1 6.1921
H6A H 0 1.12021 0.574205 0.610433 1 -1.2
H6B H 0 0.933469 0.43789 0.61177 1 -1.2
C7 C 0 1.0152 0.5501 0.6909 1 6.1921
C8 C 0 1.1143 0.6718 0.7201 1 6.1921
H8 H 0 1.19355 0.769212 0.697077 1 -1.2
C9 C 0 0.9163 0.4277 0.7208 1 6.1921
H9 H 0 0.837233 0.329763 0.697994 1 -1.2
C1S C 0 5.96853 2.86406 0.73234 0.1363(14) 15.0(27)
H1S H 0 6.059052 2.864041 0.7183312 0.1363(14) 18.0
H2S H 0 5.890563 2.816325 0.7075238 0.1363(14) 18.0
C2S C 0 5.961254 2.916856 0.7827942 0.1363(14) 15.0(27)
H3S H 0 5.872087 2.910197 0.7958121 0.1363(14) 18.0
H4S H 0 6.048693 2.962506 0.8087035 0.1363(14) 18.0


# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag


# C8     C8        1.4108(1)       .     10_556       no                                                           
# C9     C9        1.3778(1)       .     10_556       no




# Cl1    O1         1.3686     .     3_655      no
# Cl1    O1         1.3686      .     5_665      no
Fe1 N1 2.1705(1) . . no
N1 N5 1.3604(1) . . no
N1 C2 1.2993(1) . . no
N3 N4 1.3477(1) . . no
N3 C2 1.3208(1) . . no
N3 C6 1.4655(1) . . no
N4 N5 1.3181(1) . . no
C6 C7 1.5266(1) . . no
C7 C8 1.3660(1) . . no
C7 C9 1.3779(1) . . no
C2 H2 1.09 . . no
C6 H6A 1.09 . . no
C6 H6B 1.09 . . no
C8 H8 1.09 . . no
C9 H9 1.09 . . no
C1S C2S 1.3318 . . no
C1S H1S 1.01 . . no
C1S H2S 0.93 . . no
C2S H3S 0.96 . . no
C2S H4S 1.00 . . no
Cl1 O1 1.3686(1) . . no
Cl1 O2 1.3683(1) . . no
Cl1B O1 1.3527(1) . . no
Cl1B O2B 1.3848(1) . . no
# Cl1B   O1          1.3527     .     3_655      no                                    
# Cl1B   O1          1.3527     .     5_665      no







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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag







N1 Fe1 N1 91.00 . . 3_555 no
N1 Fe1 N1 180.00 . . 7_555 no
N1 Fe1 N1 89.00 . . 9_555 no
Fe1 N1 N5 122.91 . . . no
Fe1 N1 C2 130.12 . . . no
N5 N1 C2 106.30 . . . no
N4 N3 C2 108.35 . . . no
N4 N3 C6 119.99 . . . no
C2 N3 C6 131.27 . . . no
N3 N4 N5 106.01 . . . no
N1 N5 N4 109.41 . . . no
N1 C2 N3 109.79 . . . no
N3 C6 C7 112.18 . . . no
C6 C7 C8 121.18 . . . no
C6 C7 C9 119.90 . . . no
C8 C7 C9 118.92 . . . no
C7 C8 C8 120.29 . . 10_556 no
C7 C9 C9 120.79 . . 10_556 no
N1 C2 H2 125 . . . no
N3 C2 H2 125 . . . no
N3 C6 H6A 109 . . . no
N3 C6 H6B 109 . . . no
C7 C6 H6A 109 . . . no
C7 C6 H6B 109 . . . no
H6A C6 H6B 108 . . . no
C7 C8 H8 120 . . . no
H8 C8 C8 120 . . 10_555 no
C7 C9 H9 120 . . . no
H9 C9 C9 120 . . 10_555 no
C2S C1S H1S 123 . . . no
C2S C1S H2S 125 . . . no
H1S C1S H2S 112 . . . no
C1S C2S H3S 121 . . . no
C1S C2S H4S 121 . . . no
H3S C2S H4S 118 . . . no
O1 Cl1 O2 102.04 . . . no
O1 Cl1 O1 115.77 . . 3_655 no
O1 Cl1B O2B 98.32 . . . no
O1 Cl1B O1 117.94 . . 3_655 no



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






N1 Fe1 N1 N5 107.46 3_555 . . . no
N1 Fe1 N1 C2 -61.78 3_555 . . . no
N1 Fe1 N1 N5 16.44 5_555 . . . no
N1 Fe1 N1 C2 -152.80 5_555 . . . no
N1 Fe1 N1 N5 -72.54 9_555 . . . no
N1 Fe1 N1 C2 118.22 9_555 . . . no
N1 Fe1 N1 N5 -163.56 11_555 . . . no
N1 Fe1 N1 C2 27.20 11_555 . . . no
Fe1 N1 N5 N4 -173.98 . . . . no
C2 N1 N5 N4 -2.54 . . . . no
Fe1 N1 C2 N3 170.89 . . . . no
N5 N1 C2 N3 0.30 . . . . no
C2 N3 N4 N5 -3.48 . . . . no
C6 N3 N4 N5 -177.18 . . . . no
N4 N3 C2 N1 1.99 . . . . no
C6 N3 C2 N1 174.72 . . . . no
N4 N3 C6 C7 -55.69 . . . . no
C2 N3 C6 C7 132.28 . . . . no
N3 N4 N5 N1 3.69 . . . . no
N3 C6 C7 C8 -64.60 . . . . no
N3 C6 C7 C9 115.34 . . . . no
C6 C7 C8 C8 179.57 . . . 10_555 no
C9 C7 C8 C8 -0.36 . . . 10_555 no
C6 C7 C9 C9 -179.57 . . . 10_555 no
C8 C7 C9 C9 0.36 . . . 10_555 no
Fe1 N1 C2 H2 -10 . . . . no
N5 N1 C2 H2 180 . . . . no
N4 N3 C2 H2 -177 . . . . no
C6 N3 C2 H2 -5 . . . . no
N4 N3 C6 H6A -177 . . . . no
N4 N3 C6 H6B 65 . . . . no
C2 N3 C6 H6A 11 . . . . no
C2 N3 C6 H6B -107 . . . . no
H6A C6 C7 C8 57 . . . . no
H6A C6 C7 C9 -123 . . . . no
H6B C6 C7 C8 174 . . . . no
H6B C6 C7 C9 -6 . . . . no
C6 C7 C8 H8 0 . . . . no
C9 C7 C8 H8 180 . . . . no
C6 C7 C9 H9 0 . . . . no
C8 C7 C9 H9 -180 . . . . no
C7 C8 C8 H8 -180 . . 10_555 10_555 no
C7 C9 C9 H9 -180 . . 10_555 10_555 no





















_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_ccp1_CH4
_database_code_depnum_ccdc_archive 'CCDC 1473651'
_audit_update_record             
;
2016-04-12 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H30 Fe N24, 2(Cl O4), 0.78(C H4)'
_chemical_formula_structural     'Fe (C10 H10 N8)3, 2(ClO4) 0.78(CH4)'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C30.78 H33.12 Cl2 Fe N24 O8'
_chemical_formula_weight         994.04
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Hexagonal
_space_group_name_H-M_alt        P63/m
_space_group_name_Hall           -P_6c
_symmetry_Int_Tables_number      176

loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'

_cell_length_a                   10.5426(2)
_cell_length_b                   10.5426(2)
_cell_length_c                   23.6588(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2277.30(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4497(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1019.6



# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              10
# perpendicular to equatorial plane
_pd_spec_size_equat              1
# parallel to scattering vector  in transmission
_pd_spec_size_thick              ?
# parallel to scattering vector  in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                '1 mm borosilicate capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'visual estimate, prisms'
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.
_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; Diamond Light Source
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_radiation_wavelength     0.799933
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  'BEamline BL04, ALBA'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 ?
_diffrn_detector_type            '40 degrees Mythen'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;
;
_pd_meas_number_of_points        6850
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.003

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_number            628

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_data_reduction        'Topas (Coelho, 2003)'
_computing_structure_solution    'Topas (Coelho, 2003)'
_computing_structure_refinement  'Topas (Coelho, 2003)'
_computing_publication_material  
'enCifer (Cambridge Crystallographic Data Centre, 2004)'

#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; 
The structure solution was obtained by global optimisation using the
DASH structure solution program.  The internal coordinate 
description of the molecule was constructed from standard bond
lengths, bond angles and bond torsions where appropriate.
 The structure was refined against data in the range 
2.0 to 40.0° 2θ (628 reflections).
;

# The next three items are given as text
_pd_proc_ls_profile_function     
;   
Fundamental parameters with axial divergence correction
;
_pd_proc_ls_background_function  
;
Chebyshev polynomial
;
_pd_proc_ls_pref_orient_corr     
; 
A spherical harmonics-based preferred orientation correction 
was applied with Topas during the Rietveld refinement.
;

_pd_proc_ls_prof_R_wp_factor     0.01073
_pd_proc_ls_prof_R_wp_dash_factor 0.14669
_pd_proc_ls_prof_wR_expected     0.00899

_refine_special_details          'powder data'

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     55
_refine_ls_number_restraints     64
_refine_ls_number_constraints    0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.285

_refine_ls_R_I_factor            ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?



# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id       ccp_1_CH4_6bar_fsum.xye

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe 0 1 1 0.5 1 4.03(21)
O1 O 0 0.802 0.4505 0.4954 1 11.31(48)
Cl1 Cl 0 0.6666667 0.3333333 0.5075 0.605(12) 8.9(11)
O2 O 0 0.6666667 0.3333333 0.5655 0.605(12) 8.9(11)
Cl1b Cl 0 0.6666667 0.3333333 0.4871 0.395(12) 5.0(16)
O2b O 0 0.6666667 0.3333333 0.4284 0.395(12) 5.0(16)
N1 N 0 0.95445 0.81195 0.55218 1 7.46(22)
C2 C 0 1.0339 0.7515 0.562 1 7.46(22)
H2 H 0 1.1345 0.777257 0.539823 1 8.95(27)
N3 N 0 0.9733 0.6528 0.6027 1 7.46(22)
N4 N 0 0.8471 0.6465 0.6184 1 7.46(22)
N5 N 0 0.8391 0.7484 0.5887 1 7.46(22)
C6 C 0 1.0125 0.548 0.6262 1 7.46(22)
H6A H 0 1.11997 0.574147 0.610467 1 8.95(27)
H6B H 0 0.933642 0.43813 0.611802 1 8.95(27)
C7 C 0 1.0152 0.5501 0.6909 1 7.46(22)
C8 C 0 1.1143 0.6718 0.7201 1 7.46(22)
H8 H 0 1.19337 0.768989 0.69713 1 8.95(27)
C9 C 0 0.9163 0.4277 0.7208 1 7.46(22)
H9 H 0 0.837414 0.329987 0.698047 1 8.95(27)
C1S C 0 -0.00915 0.1043 0.2898 0.1300(43) 3
H1S H 0 -0.09502 0.01214 0.26561 0.1300(43) 3.6
H2S H 0 -0.03372 0.1929 0.29144 0.1300(43) 3.6
H3S H 0 -0.00519 0.0683 0.33262 0.1300(43) 3.6
H4S H 0 0.09692 0.14294 0.26925 0.1300(43) 3.6

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag


# C8     C8        1.4148(1)       .     10_556       no                                                           
# C9     C9        1.3817(1)       .     10_556       no





# Cl1    O1       1.3715     .     3_655      no
# Cl1    O1       1.3715      .     5_665      no
Fe1 N1 2.1756(1) . . no
N1 N5 1.3636(1) . . no
N1 C2 1.3021(1) . . no
N3 N4 1.3506(1) . . no
N3 C2 1.3241(1) . . no
N3 C6 1.4688(1) . . no
N4 N5 1.3212(1) . . no
C6 C7 1.5309(1) . . no
C7 C8 1.3691(1) . . no
C7 C9 1.3810(1) . . no
C2 H2 1.09 . . no
C6 H6A 1.09 . . no
C6 H6B 1.09 . . no
C8 H8 1.09 . . no
C9 H9 1.09 . . no
C1S H1S 1.10 . . no
C1S H2S 1.09 . . no
C1S H3S 1.09 . . no
C1S H4S 1.09 . . no
Cl1 O1 1.3715(1) . . no
Cl1 O2 1.3722(1) . . no
Cl1B O1 1.3556(1) . . no
Cl1B O2B 1.3888(1) . . no
# Cl1B   O1          1.3556     .     3_655      no                                    
# Cl1B   O1          1.3556     .     5_665      no







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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag








N1 Fe1 N1 90.97 . . 3_555 no
N1 Fe1 N1 180.00 . . 7_555 no
N1 Fe1 N1 89.03 . . 9_555 no
Fe1 N1 N5 122.93 . . . no
Fe1 N1 C2 130.12 . . . no
N5 N1 C2 106.28 . . . no
N4 N3 C2 108.36 . . . no
N4 N3 C6 119.98 . . . no
C2 N3 C6 131.28 . . . no
N3 N4 N5 106.00 . . . no
N1 N5 N4 109.43 . . . no
N1 C2 N3 109.80 . . . no
N3 C6 C7 112.20 . . . no
C6 C7 C8 121.20 . . . no
C6 C7 C9 119.92 . . . no
C8 C7 C9 118.88 . . . no
C7 C8 C8 120.30 . . 10_556 no
C7 C9 C9 120.81 . . 10_556 no
N1 C2 H2 125 . . . no
N3 C2 H2 125 . . . no
N3 C6 H6A 109 . . . no
N3 C6 H6B 109 . . . no
C7 C6 H6A 109 . . . no
C7 C6 H6B 109 . . . no
H6A C6 H6B 108 . . . no
C7 C8 H8 120 . . . no
H8 C8 C8 120 . . 10_555 no
C7 C9 H9 120 . . . no
H9 C9 C9 120 . . 10_555 no
H1S C1S H2S 109 . . . no
H1S C1S H3S 109 . . . no
H1S C1S H4S 110 . . . no
H2S C1S H3S 109 . . . no
H2S C1S H4S 110 . . . no
H3S C1S H4S 109 . . . no
O1 Cl1 O2 102.05 . . . no
O1 Cl1 O1 115.76 . . 3_655 no
O1 Cl1B O2B 98.33 . . . no
O1 Cl1B O1 117.94 . . 3_655 no



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






N1 Fe1 N1 N5 107.43 3_555 . . . no
N1 Fe1 N1 C2 -61.80 3_555 . . . no
N1 Fe1 N1 N5 16.44 5_555 . . . no
N1 Fe1 N1 C2 -152.79 5_555 . . . no
N1 Fe1 N1 N5 -72.57 9_555 . . . no
N1 Fe1 N1 C2 118.20 9_555 . . . no
N1 Fe1 N1 N5 -163.56 11_555 . . . no
N1 Fe1 N1 C2 27.21 11_555 . . . no
Fe1 N1 N5 N4 -173.98 . . . . no
C2 N1 N5 N4 -2.54 . . . . no
Fe1 N1 C2 N3 170.89 . . . . no
N5 N1 C2 N3 0.30 . . . . no
C2 N3 N4 N5 -3.48 . . . . no
C6 N3 N4 N5 -177.18 . . . . no
N4 N3 C2 N1 1.99 . . . . no
C6 N3 C2 N1 174.71 . . . . no
N4 N3 C6 C7 -55.67 . . . . no
C2 N3 C6 C7 132.30 . . . . no
N3 N4 N5 N1 3.69 . . . . no
N3 C6 C7 C8 -64.60 . . . . no
N3 C6 C7 C9 115.34 . . . . no
C6 C7 C8 C8 179.57 . . . 10_555 no
C9 C7 C8 C8 -0.36 . . . 10_555 no
C6 C7 C9 C9 -179.57 . . . 10_555 no
C8 C7 C9 C9 0.36 . . . 10_555 no
Fe1 N1 C2 H2 -10 . . . . no
N5 N1 C2 H2 180 . . . . no
N4 N3 C2 H2 -177 . . . . no
C6 N3 C2 H2 -5 . . . . no
N4 N3 C6 H6A -177 . . . . no
N4 N3 C6 H6B 65 . . . . no
C2 N3 C6 H6A 11 . . . . no
C2 N3 C6 H6B -107 . . . . no
H6A C6 C7 C8 57 . . . . no
H6A C6 C7 C9 -123 . . . . no
H6B C6 C7 C8 174 . . . . no
H6B C6 C7 C9 -6 . . . . no
C6 C7 C8 H8 0 . . . . no
C9 C7 C8 H8 180 . . . . no
C6 C7 C9 H9 0 . . . . no
C8 C7 C9 H9 -180 . . . . no
C7 C8 C8 H8 -180 . . 10_555 10_555 no
C7 C9 C9 H9 -180 . . 10_555 10_555 no





















_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_ccp2_co2
_database_code_depnum_ccdc_archive 'CCDC 1473652'
_audit_update_record             
;
2016-04-12 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

# 5. CHEMICAL DATA


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H30 N24 Fe, 2(BF4) 1.04(CO2)'
_chemical_formula_structural     'Fe (C10 H10 N8)3, 2(BF4) 1.04(CO2)'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'B2 C31.044 F8 Fe1 H30 N24 O2.088'
_chemical_formula_weight         1002.161559
_chemical_melting_point          ?
_chemical_compound_sour          'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.017 0.010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.001 0.001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Hexagonal
_space_group_name_H-M_alt        P63/m
_space_group_name_Hall           -P_6c
_symmetry_Int_Tables_number      176
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'

_cell_length_a                   10.57127(10)
_cell_length_b                   10.57127(10)
_cell_length_c                   23.48130(37)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2272.517(57)

_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4646(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1017.9

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              10
# perpendicular to equatorial plane
_pd_spec_size_equat              1
# parallel to scattering vector  in transmission
_pd_spec_size_thick              ?
# parallel to scattering vector  in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                '1 mm quartz capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'visual estimate, prisms'
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.
_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?


#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ALBA
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_radiation_wavelength     0.799933
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  'BEamline BL04, ALBA'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 ?
_diffrn_detector_type            '40 degrees Mythen'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;


;

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.
_pd_meas_number_of_points        6850
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.003

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_number            628

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_data_reduction        'Topas (Coelho, 2003)'
_computing_structure_solution    'Topas (Coelho, 2003)'
_computing_structure_refinement  'Topas (Coelho, 2003)'
_computing_publication_material  
'enCifer (Cambridge Crystallographic Data Centre, 2004)'

#==============================================================================



# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; The structure solution was obtained by global optimisation using the
TOPAS structure solution program.  The internal coordinate 
description of the molecule was constructed from standard bond
lengths, bond angles and bond torsions where appropriate.
The structure was refined against data in the range 
2.0 to 40.0° 2θ (565 reflections).  
;

# The next three items are given as text

_pd_proc_ls_profile_function     
;   
Fundamental parameters with axial divergence correction
;
_pd_proc_ls_background_function  
;Chebyshev polynomial
;
_pd_proc_ls_pref_orient_corr     Spherical_Harmonics

_pd_proc_ls_prof_R_wp_factor     0.03131
_pd_proc_ls_prof_R_wp_dash_factor 0.15339
_pd_proc_ls_prof_wR_expected     0.00957

_refine_special_details          'powder data'

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     62
_refine_ls_number_restraints     56
_refine_ls_number_constraints    1

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   3.271

_refine_ls_R_I_factor            ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?



# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id       ccp_2_co2_6bar_fsum.xye

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe 0 1 1 0.5 1 3.80(14)
F1 F 0 0.6666667 0.3333333 0.578447 0.4677(40) 9.84(32)
Ba B 0 0.6666667 0.3333333 0.518371 0.4677(40) 9.84(32)
F2 F 0 0.655261 0.198037 0.506056 0.4677(40) 9.84(32)
F1b F 0 0.6666667 0.3333333 0.429087 0.5323(40) 9.84(32)
Bb B 0 0.6666667 0.3333333 0.489085 0.5323(40) 9.84(32)
F2b F 0 0.541366 0.198282 0.499924 0.5323(40) 9.84(32)
N1 N 0 0.95234 0.80768 0.55433 1 6.60(16)
C2 C 0 1.03317 0.75211 0.56683 1 6.60(16)
H2 H 0 1.14202 0.780113 0.552399 1 7.92(19)
N3 N 0 0.96958 0.65024 0.60396 1 6.60(16)
N4 N 0 0.84089 0.63577 0.61763 1 6.60(16)
N5 N 0 0.82266 0.73 0.58827 1 6.60(16)
C6 C 0 1.02429 0.54743 0.62699 1 6.60(16)
H6A H 0 1.13756 0.587006 0.615096 1 7.92(19)
H6B H 0 0.955836 0.436096 0.611709 1 7.92(19)
C7 C 0 1.020158019(35) 0.548254695(29) 0.691356194(13) 1 6.60(16)
C8 C 0 1.10823786(12) 0.675918248(53) 0.720719689(13) 1 6.60(16)
H8 H 0 1.17254 0.77754 0.697392 1 7.92(19)
C9 C 0 0.92057502(11) 0.424746793(65) 0.720319401(14) 1 6.60(16)
H9 H 0 0.844379 0.327544 0.696649 1 7.92(19)
O2S O 0 0.07151694 0.1181834 0.2416963 0.1740(17) 5.3003
C1S C 0 0.07157687 0.02606326 0.2148751 0.1740(17) 5.3003
O1S O 0 0.0716368 -0.06605688 0.1880539 0.1740(17) 5.3003


#==============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

#C8     C8        1.3751(1)      10_556  .     no   
#C9     C9        1.3939(1)      10_556  .     no





Fe1 N1 2.2339(1) . . no
N1 N5 1.4363(1) . . no
N1 C2 1.2897(1) . . no
N3 N4 1.3301(1) . . no
N3 C2 1.2837(1) . . no
N3 C6 1.5610(1) . . no
N4 N5 1.3026(1) . . no
C6 C7 1.5122(1) . . no
C7 C8 1.3810(1) . . no
C7 C9 1.3788(1) . . no
C2 H2 1.09 . . no
C6 H6A 1.09 . . no
C6 H6B 1.09 . . no
C8 H8 1.09 . . no
C9 H9 1.09 . . no
O1S C1S 1.160 . . no
O2S C1S 1.160 . . no
Ba F1 1.4107(1) . . no
Ba F2 1.4040(1) . . no
Bb F1B 1.4088(1) . . no
Bb F2B 1.4023(1) . . no





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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag








N1 Fe1 N1 90.62 . . 3.765 no
N1 Fe1 N1 180.00 . . 7.776 no
N1 Fe1 N1 89.38 . . 9.566 no
Fe1 N1 N5 123.62 . . . no
Fe1 N1 C2 130.18 . . . no
N5 N1 C2 105.88 . . . no
N4 N3 C2 109.69 . . . no
N3 N4 N5 108.56 . . . no
N3 C6 C7 108.69 . . . no
C8 C7 C9 120.11 . . . no
N4 N3 C6 123.37 . . . no
N1 N5 N4 105.49 . . . no
C6 C7 C8 119.83 . . . no
C2 N3 C6 126.76 . . . no
N1 C2 N3 110.39 . . . no
C6 C7 C9 119.88 . . . no
C7 C8 C8 119.95 . . 10_556 no
C7 C9 C9 115.71 . . 10_556 no
N1 C2 H2 131 . . . no
N3 C6 H6B 111 . . . no
H6A C6 H6B 110 . . . no
C7 C9 H9 119.74 . . . no
N3 C2 H2 119 . . . no
C7 C6 H6A 106 . . . no
C7 C8 H8 119.75 . . . no
H9 C9 C9 123.10 . . 10_556 no
N3 C6 H6A 111 . . . no
C7 C6 H6B 109 . . . no
H8 C8 C8 115.12 . . 10_556 no
O1S C1S O2S 180.00 . . . no
F1 BA F2 100.46 . . . no
F2 BA F2 116.78 . . 3_655 no
F1B BB F2B 101.89 . . . no
F2B BB F2B 115.87 . . 3_655 no


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



C2 N1 N5 N4 0.08 . . . . no
Fe1 N1 C2 N3 173.68 . . . . no
N4 N3 C2 N1 5.17 . . . . no
C2 N3 C6 C7 129.90 . . . . no
Fe1 N1 N5 N4 -174.01 . . . . no
C6 N3 N4 N5 -175.04 . . . . no
N4 N3 C2 N1 -0.29 . . . . no
N5 N1 C2 N3 0.13 . . . . no
N4 N3 C6 C7 -55.54 . . . . no
N3 C6 C7 C8 -63.76 . . . . no
N3 C6 C7 C9 111.22 . . . . no
C9 C7 C8 C8 7.15 . . . 10.556 no
C6 C7 C9 C9 177.91 . . . 10.556 no
N5 N1 C2 H2 -178 . . . . no
N4 N3 C2 H2 178 . . . . no
N4 N3 C6 H6A -172 . . . . no
N4 N3 C6 H6B 65 . . . . no
C2 N3 C6 H6B -110 . . . . no
H6A C6 C7 C8 56 . . . . no
H6B C6 C7 C8 175 . . . . no
H6B C6 C7 C9 -10 . . . . no
C9 C7 C8 H8 -169.21 . . . . no
C6 C7 C9 H9 -0.77 . . . . no
C7 C8 C8 H8 -176.34 . . 10.556 10.556 no
C7 C9 C9 H9 -178.67 . . 10.556 10.556 no






_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_ccp2_C2H4
_database_code_depnum_ccdc_archive 'CCDC 1473653'
_audit_update_record             
;
2016-04-12 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

# 5. CHEMICAL DATA


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H30 Fe N24, 2(B F4), 0.90(C2 H4)'
_chemical_formula_structural     'Fe (C10 H10 N8)3, 2(BF4) 0.9(C2H4)'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C31.80 H33.60 B2 F8 Fe N24'
_chemical_formula_weight         981.50
_chemical_melting_point          ?
_chemical_compound_sour          'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.017 0.010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.001 0.001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Hexagonal
_space_group_name_H-M_alt        P63/m
_space_group_name_Hall           -P_6c
_symmetry_Int_Tables_number      176
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'

_cell_length_a                   10.572810(77)
_cell_length_b                   10.572810(77)
_cell_length_c                   23.49996(33)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2274.985(46)

_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4328(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000.8

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              10
# perpendicular to equatorial plane
_pd_spec_size_equat              1
# parallel to scattering vector  in transmission
_pd_spec_size_thick              ?
# parallel to scattering vector  in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                '1 mm quartz capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'visual estimate, prisms'
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.
_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?


#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ALBA
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_radiation_wavelength     0.799933
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  'BEamline BL04, ALBA'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 ?
_diffrn_detector_type            '40 degrees Mythen'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;


;

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.
_pd_meas_number_of_points        6850
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.003

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_number            628

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_data_reduction        'Topas (Coelho, 2003)'
_computing_structure_solution    'Topas (Coelho, 2003)'
_computing_structure_refinement  'Topas (Coelho, 2003)'
_computing_publication_material  
'enCifer (Cambridge Crystallographic Data Centre, 2004)'

#==============================================================================



# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; The structure solution was obtained by global optimisation using the
TOPAS structure solution program.  The internal coordinate 
description of the molecule was constructed from standard bond
lengths, bond angles and bond torsions where appropriate.
The structure was refined against data in the range 
3.0 to 40.0° 2θ (628 reflections).  
;

# The next three items are given as text

_pd_proc_ls_profile_function     
;   
Fundamental parameters with axial divergence correction
;
_pd_proc_ls_background_function  
;Chebyshev polynomial
;
_pd_proc_ls_pref_orient_corr     Spherical_Harmonics

_pd_proc_ls_prof_R_wp_factor     0.03566
_pd_proc_ls_prof_wR_factor       0.03566
_pd_proc_ls_prof_R_wp_dash_factor 0.15761
_pd_proc_ls_prof_wR_expected     0.00954

_refine_special_details          'powder data'

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     61
_refine_ls_number_restraints     56
_refine_ls_number_constraints    1

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   3.738

_refine_ls_R_I_factor            ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?



# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id       ccp_2_C2H4_6bar_fsum.xye

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe 0 1 1 0.5 1 4.19(15)
F1 F 0 0.6666667 0.3333333 0.578447 0.4480(40) 9.95(31)
Ba B 0 0.6666667 0.3333333 0.518371 0.4480(40) 9.95(31)
F2 F 0 0.655261 0.198037 0.506056 0.4480(40) 9.95(31)
F1b F 0 0.6666667 0.3333333 0.429087 0.5520(40) 9.95(31)
Bb B 0 0.6666667 0.3333333 0.489085 0.5520(40) 9.95(31)
F2b F 0 0.541366 0.198282 0.499924 0.5520(40) 9.95(31)
N1 N 0 0.95234 0.80768 0.55433 1 6.17(17)
C2 C 0 1.03317 0.75211 0.56683 1 6.17(17)
H2 H 0 1.142 0.780107 0.552402 1 -1.2
N3 N 0 0.96958 0.65024 0.60396 1 6.17(17)
N4 N 0 0.84089 0.63577 0.61763 1 6.17(17)
N5 N 0 0.82266 0.73 0.58827 1 6.17(17)
C6 C 0 1.02429 0.54743 0.62699 1 6.17(17)
H6A H 0 1.13754 0.586999 0.615098 1 -1.2
H6B H 0 0.955851 0.43612 0.611712 1 -1.2
C7 C 0 1.0203 0.54811 0.69124 1 6.17(17)
C8 C 0 1.10996 0.67553 0.7207 1 6.17(17)
H8 H 0 1.18216 0.775056 0.697424 1 -1.2
C9 C 0 0.91946 0.42512 0.72046 1 6.17(17)
H9 H 0 0.839235 0.329562 0.697048 1 -1.2
C2S C 0 5.978282 2.904003 0.7771553 0.1498(24) 2.4(17)
C1S C 0 5.98681 2.856103 0.7256777 0.1498(24) 2.4(17)
H1S H 0 6.078697 2.861664 0.7105627 0.1498(24) -1.2
H2S H 0 5.908957 2.807159 0.7009947 0.1498(24) -1.2
H3S H 0 5.888095 2.892109 0.7911627 0.1498(24) -1.2
H4S H 0 6.065944 2.951373 0.8027936 0.1498(24) -1.2


#==============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

#C8     C8        1.3771(1)      10_556  .     no   
#C9     C9        1.3884(1)      10_556  .     no






Fe1 N1 2.2347(1) . . no
N1 N5 1.4368(1) . . no
N1 C2 1.2899(1) . . no
N3 N4 1.3303(1) . . no
N3 C2 1.2843(1) . . no
N3 C6 1.5614(1) . . no
N4 N5 1.3030(1) . . no
C6 C7 1.5106(1) . . no
C7 C8 1.3841(1) . . no
C7 C9 1.3830(1) . . no
C2 H2 1.09 . . no
C6 H6A 1.09 . . no
C6 H6B 1.09 . . no
C8 H8 1.09 . . no
C9 H9 1.09 . . no
C1S C2S 1.3318(1) . . no
C1S H1S 1.01 . . no
C1S H2S 0.93 . . no
C2S H3S 0.96 . . no
C2S H4S 1.00 . . no
Ba F1 1.4118(1) . . no
Ba F2 1.4043(1) . . no
Bb F1B 1.4100(1) . . no
Bb F2B 1.4025(1) . . no





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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag










N1 Fe1 N1 90.59 . . 3.765 no
N1 Fe1 N1 180.00 . . 7.776 no
N1 Fe1 N1 89.41 . . 9.566 no
Fe1 N1 N5 123.63 . . . no
Fe1 N1 C2 130.18 . . . no
N5 N1 C2 105.87 . . . no
N4 N3 C2 109.69 . . . no
N3 N4 N5 108.54 . . . no
N3 C6 C7 108.80 . . . no
C8 C7 C9 120.11 . . . no
N4 N3 C6 123.36 . . . no
N1 N5 N4 105.50 . . . no
C6 C7 C8 119.83 . . . no
C2 N3 C6 126.77 . . . no
N1 C2 N3 110.39 . . . no
C6 C7 C9 120.13 . . . no
C7 C8 C8 120.01 . . 10_556 no
C7 C9 C9 119.77 . . 10_556 no
N1 C2 H2 131 . . . no
N3 C6 H6B 111 . . . no
H6A C6 H6B 110 . . . no
C7 C9 H9 120 . . . no
N3 C2 H2 119 . . . no
C7 C6 H6A 106 . . . no
C7 C8 H8 120 . . . no
H9 C9 C9 120 . . 10_556 no
N3 C6 H6A 111 . . . no
C7 C6 H6B 109 . . . no
H8 C8 C8 120 . . 10_556 no
C2S C1S H1S 123 . . . no
C2S C1S H2S 125 . . . no
H1S C1S H2S 112 . . . no
C1S C2S H3S 121 . . . no
C1S C2S H4S 121 . . . no
H3S C2S H4S 118 . . . no
F1 BA F2 101.89 . . . no
F2 BA F2 115.87 . . 3_655 no
F1B BB F2B 100.46 . . . no
F2B BB F2B 116.78 . . 3_655 no


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


C2 N1 N5 N4 0.08 . . . . no
Fe1 N1 C2 N3 173.68 . . . . no
N4 N3 C2 N1 -0.29 . . . . no
C2 N3 C6 C7 129.90 . . . . no
Fe1 N1 N5 N4 -174.00 . . . . no
C6 N3 N5 N4 -175.04 . . . . no
N4 N3 C2 N1 -0.29 . . . . no
N5 N1 C2 N3 0.13 . . . . no
N4 N3 C6 C7 -55.54 . . . . no
N3 C6 C7 C8 -63.76 . . . . no
N3 C6 C7 C9 110.38 . . . . no
C9 C7 C8 C8 7.05 . . . 10.556 no
C6 C7 C9 C9 178.02 . . . 10.556 no
N5 N1 C2 H2 -178 . . . . no
N4 N3 C2 H2 178 . . . . no
N4 N3 C6 H6A -172 . . . . no
N4 N3 C6 H6B 65 . . . . no
C2 N3 C6 H6B -110 . . . . no
H6A C6 C7 C8 55 . . . . no
H6B C6 C7 C8 174 . . . . no
H6B C6 C7 C9 -11 . . . . no
C9 C7 C8 H8 -174 . . . . no
C6 C7 C9 H9 -0.77 . . . . no
C7 C8 C8 H8 179 . . 10.556 10.556 no
C7 C9 C9 H9 179 . . 10.556 10.556 no






_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_ccp2_CH4
_database_code_depnum_ccdc_archive 'CCDC 1473654'
_audit_update_record             
;
2016-04-12 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;

# 5. CHEMICAL DATA


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H30 Fe N24, 2(B F4), 0.84(CH4)'
_chemical_formula_structural     'Fe (C10 H10 N8)3, 2(BF4) 0.84(CH4)'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C30.84 H33.36 B2 F8 Fe N24'
_chemical_formula_weight         969.73
_chemical_melting_point          ?
_chemical_compound_sour          'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.017 0.010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.001 0.001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'




#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Hexagonal
_space_group_name_H-M_alt        P63/m
_space_group_name_Hall           -P_6c
_symmetry_Int_Tables_number      176
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'

_cell_length_a                   10.56810(7)
_cell_length_b                   10.56810(7)
_cell_length_c                   23.4989(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2272.85(4)

_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4170(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             988.8

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              10
# perpendicular to equatorial plane
_pd_spec_size_equat              1
# parallel to scattering vector  in transmission
_pd_spec_size_thick              ?
# parallel to scattering vector  in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                '1 mm quartz capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'visual estimate, prisms'
_pd_char_colour                  white

# The following three fields describe the preparation of the specimen.   
# The cooling rate is in K/min.  The pressure at which the sample was  
# prepared is in kPa.  The temperature of preparation is in K.
_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             298

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?


#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ALBA
;

_diffrn_ambient_temperature      298
_diffrn_source                   synchrotron
_diffrn_radiation_wavelength     0.799933
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  'BEamline BL04, ALBA'
_diffrn_radiation_monochromator  ?
_diffrn_detector                 ?
_diffrn_detector_type            '40 degrees Mythen'
_pd_meas_scan_method             cont
_pd_meas_special_details         
;


;

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.
_pd_meas_number_of_points        6850
_pd_meas_2theta_range_min        3.0
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.003

_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_number            628

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_data_reduction        'Topas (Coelho, 2003)'
_computing_structure_solution    'Topas (Coelho, 2003)'
_computing_structure_refinement  'Topas (Coelho, 2003)'
_computing_publication_material  
'enCifer (Cambridge Crystallographic Data Centre, 2004)'

#==============================================================================



# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; The structure solution was obtained by global optimisation using the
TOPAS structure solution program.  The internal coordinate 
description of the molecule was constructed from standard bond
lengths, bond angles and bond torsions where appropriate.
The structure was refined against data in the range 
2.0 to 40.0° 2θ (565 reflections).  
;

# The next three items are given as text

_pd_proc_ls_profile_function     
;   
Fundamental parameters with axial divergence correction
;
_pd_proc_ls_background_function  
;Chebyshev polynomial
;
_pd_proc_ls_pref_orient_corr     Spherical_Harmonics

_pd_proc_ls_prof_R_wp_factor     0.03289
_pd_proc_ls_prof_R_wp_dash_factor 0.13632
_pd_proc_ls_prof_wR_expected     0.00956

_refine_special_details          'powder data'

_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     55
_refine_ls_number_restraints     64
_refine_ls_number_constraints    0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   3.442

_refine_ls_R_I_factor            ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?



# Each refinement must be accompanied by a listing of the powder data
# in CIF format.  Each listing should be sent as a separate file consisting 
# of one data block containing a single powder profile. The value of 
# _pd_block_diffractogram_id is used to associate each refinement with 
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. 

_pd_block_diffractogram_id       ccp_2_CH4_6bar_fsum.xye

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe 0 1 1 0.5 1 4.78(14)
F1 F 0 0.6666667 0.3333333 0.578447 0.44777 15.85(41)
Ba B 0 0.6666667 0.3333333 0.518371 0.44777 15.85(41)
F2 F 0 0.655261 0.198037 0.506056 0.44777 15.85(41)
F1b F 0 0.6666667 0.3333333 0.429087 0.55223 15.85(41)
Bb B 0 0.6666667 0.3333333 0.489085 0.55223 15.85(41)
F2b F 0 0.541366 0.198282 0.499924 0.55223 15.85(41)
N1 N 0 0.95234 0.80768 0.55433 1 4.88(13)
C2 C 0 1.03317 0.75211 0.56683 1 4.88(13)
H2 H 0 1.14204 0.780118 0.552396 1 -1.5
N3 N 0 0.96958 0.65024 0.60396 1 4.88(13)
N4 N 0 0.84089 0.63577 0.61763 1 4.88(13)
N5 N 0 0.82266 0.73 0.58827 1 4.88(13)
C6 C 0 1.02429 0.54743 0.62699 1 4.88(13)
H6A H 0 1.13759 0.587016 0.615093 1 -1.5
H6B H 0 0.955823 0.436075 0.611706 1 -1.5
C7 C 0 1.0203 0.54811 0.69124 1 4.88(13)
C8 C 0 1.10996 0.67553 0.7207 1 4.88(13)
H8 H 0 1.18219 0.775091 0.697416 1 -1.5
C9 C 0 0.91946 0.42512 0.72046 1 4.88(13)
H9 H 0 0.839208 0.329529 0.69704 1 -1.5
C1S C 0 -0.00914000(17) 0.10419000(20) 0.289810000(84) 0.14 8
H1S H 0 -0.09497000(32) 0.01214000(42) 0.26546000(29) 0.14 -1.5
H2S H 0 -0.03378000(48) 0.19275000(57) 0.29148000(21) 0.14 -1.5
H3S H 0 -0.00523000(64) 0.06840000(39) 0.33272000(21) 0.14 -1.5
H4S H 0 0.09680000(55) 0.14293000(35) 0.26909000(28) 0.14 -1.5


#==============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

#C8     C8        1.3770(1)      10_556  .     no   
#C9     C9        1.3883(1)      10_556  .     no




Fe1 N1 2.2340(1) . . no
N1 N5 1.4364(1) . . no
N1 C2 1.2894(1) . . no
N3 N4 1.3298(1) . . no
N3 C2 1.2839(1) . . no
N3 C6 1.5607(1) . . no
N4 N5 1.3026(1) . . no
C6 C7 1.5105(1) . . no
C7 C8 1.3836(1) . . no
C7 C9 1.3825(1) . . no
C2 H2 1.09 . . no
C6 H6A 1.09 . . no
C6 H6B 1.09 . . no
C8 H8 1.09 . . no
C9 H9 1.09 . . no
C1S H1S 1.1019(1) . . no
C1S H2S 1.0904(1) . . no
C1S H3S 1.0850(1) . . no
C1S H4S 1.0954(1) . . no
Ba F1 1.4117(1) . . no
Ba F2 1.4037(1) . . no
Bb F1B 1.4099(1) . . no
Bb F2B 1.4019(1) . . no





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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag








N1 Fe1 N1 90.58 . . 3.765 no
N1 Fe1 N1 180.00 . . 7.776 no
N1 Fe1 N1 89.42 . . 9.566 no
Fe1 N1 N5 123.62 . . . no
Fe1 N1 C2 130.18 . . . no
N5 N1 C2 105.86 . . . no
N4 N3 C2 109.70 . . . no
N3 N4 N5 108.53 . . . no
N3 C6 C7 108.80 . . . no
C8 C7 C9 119.82 . . . no
N4 N3 C6 123.35 . . . no
N1 N5 N4 105.51 . . . no
C6 C7 C8 120.14 . . . no
C2 N3 C6 126.77 . . . no
N1 C2 N3 110.40 . . . no
C6 C7 C9 120.14 . . . no
C7 C8 C8 120.02 . . 10_556 no
C7 C9 C9 119.78 . . 10_556 no
N1 C2 H2 131 . . . no
N3 C6 H6B 111 . . . no
H6A C6 H6B 110 . . . no
C7 C9 H9 120 . . . no
N3 C2 H2 119 . . . no
C7 C6 H6A 106 . . . no
C7 C8 H8 120 . . . no
H9 C9 C9 120 . . 10_556 no
N3 C6 H6A 111 . . . no
C7 C6 H6B 109 . . . no
H8 C8 C8 120 . . 10_556 no
H1S C1S H2S 109.39(1) . . . no
H1S C1S H3S 109.44(1) . . . no
H1S C1S H4S 109.61(1) . . . no
H2S C1S H3S 109.44(1) . . . no
H2S C1S H4S 109.47(1) . . . no
H3S C1S H4S 109.48(1) . . . no
F1 BA F2 101.90 . . . no
F2 BA F2 115.86 . . 3_655 no
F1B BB F2B 100.47 . . . no
F2B BB F2B 116.78 . . 3_655 no


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



C2 N1 N5 N4 0.08 . . . . no
Fe1 N1 C2 N3 173.68 . . . . no
N4 N3 C2 N1 -0.29 . . . . no
C2 N3 C6 C7 129.91 . . . . no
Fe1 N1 N5 N4 -174.00 . . . . no
C6 N3 N4 N5 -175.04 . . . . no
N5 N1 C2 N3 0.13 . . . . no
N4 N3 C6 C7 -55.53 . . . . no
N3 C6 C7 C8 -64.57 . . . . no
N3 C6 C7 C9 110.38 . . . . no
C9 C7 C8 C8 7.04 . . . 10.556 no
C6 C7 C9 C9 178.02 . . . 10.556 no
N5 N1 C2 H2 -178 . . . . no
N4 N3 C2 H2 178 . . . . no
N4 N3 C6 H6A -172 . . . . no
N4 N3 C6 H6B 65 . . . . no
C2 N3 C6 H6B -110 . . . . no
H6A C6 C7 C8 55 . . . . no
H6B C6 C7 C8 178 . . . . no
H6B C6 C7 C9 -11 . . . . no
C9 C7 C8 H8 -174 . . . . no
C6 C7 C9 H9 -3 . . . . no
C7 C8 C8 H8 179 . . 10.556 10.556 no
C7 C9 C9 H9 179 . . 10.556 10.556 no






_exptl_crystal_preparation       'Magnetic properties'
