 
data_Fe_trz_hexa_420K_a
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C108 H72 Fe6 N36' 
_chemical_formula_weight          2209.11

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'  -1.1336   3.1974
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            166
_space_group_name_H-M_alt         'R -3 m :H'
_space_group_name_Hall            '-R 3 2"'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'y+2/3, x+1/3, -z+1/3'
 'x-y+2/3, -y+1/3, -z+1/3'
 '-x+2/3, -x+y+1/3, -z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 'y+1/3, x+2/3, -z+2/3'
 'x-y+1/3, -y+2/3, -z+2/3'
 '-x+1/3, -x+y+2/3, -z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-y+2/3, -x+1/3, z+1/3'
 '-x+y+2/3, y+1/3, z+1/3'
 'x+2/3, x-y+1/3, z+1/3'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 '-y+1/3, -x+2/3, z+2/3'
 '-x+y+1/3, y+2/3, z+2/3'
 'x+1/3, x-y+2/3, z+2/3'
 
_cell_length_a                    22.1736(14)
_cell_length_b                    22.1736(14)
_cell_length_c                    7.0796(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      3014.5(4)
_cell_formula_units_Z             1
_cell_measurement_temperature     273(2)
_cell_measurement_reflns_used     2933
_cell_measurement_theta_min       12.694
_cell_measurement_theta_max       123.206
 
_exptl_crystal_description        hexagonal
_exptl_crystal_colour             black
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.217          
_exptl_crystal_F_000              1128
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     6.103
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       273(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    'ImS 3.0 micro source'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'ω and φ scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             11951
_diffrn_reflns_av_unetI/netI      0.0195
_diffrn_reflns_av_R_equivalents   0.0443
_diffrn_reflns_limit_h_min        -26
_diffrn_reflns_limit_h_max        26
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        8
_diffrn_reflns_theta_min          3.987
_diffrn_reflns_theta_max          72.333
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              725
_reflns_number_gt                 698
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          725
_refine_ls_number_parameters      60
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0276
_refine_ls_R_factor_gt            0.0266
_refine_ls_wR_factor_ref          0.0986
_refine_ls_wR_factor_gt           0.0967
_refine_ls_goodness_of_fit_ref    0.945
_refine_ls_restrained_S_all       0.945
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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 0.666667 0.333333 0.833333 0.0112(3) Uani 1 12 d S T P . .
Fe2 Fe 0.666667 0.333333 0.333333 0.0119(3) Uani 1 12 d S T P . .
N1 N 0.58515(6) 0.29258(3) 0.67821(18) 0.0193(4) Uani 1 2 d S T P . .
N2 N 0.58204(6) 0.29102(3) 0.49190(18) 0.0181(4) Uani 1 2 d S T P . .
C1 C 0.40470(10) 0.20235(5) 0.6315(3) 0.0422(6) Uani 1 2 d S T P . .
C2 C 0.37882(14) 0.1766(6) 0.8058(4) 0.080(4) Uani 0.5 1 d . . P . .
H2 H 0.409567 0.181597 0.901963 0.064(13) Uiso 0.5 1 calc R . P . .
C3 C 0.35846(14) 0.1682(9) 0.4887(4) 0.080(5) Uani 0.5 1 d . . P . .
H3 H 0.374366 0.169923 0.366140 0.096 Uiso 0.5 1 calc R U P . .
C4 C 0.48058(9) 0.24029(4) 0.6024(3) 0.0313(4) Uani 1 2 d S T P . .
N4 N 0.52246(7) 0.26123(4) 0.7517(2) 0.0302(4) Uani 1 2 d S T P . .
H4N H 0.511117 0.255559 0.869229 0.036 Uiso 0.5 2 calc R U P . .
N3 N 0.51549(7) 0.25774(4) 0.4385(2) 0.0292(4) Uani 1 2 d S T P . .
H3N H 0.498881 0.249441 0.325725 0.035 Uiso 0.5 2 calc R U P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Fe1 N1 1.9119(13) 32_556 ?
Fe1 N1 1.9120(13) 2_655 ?
Fe1 N1 1.9121(13) . ?
Fe1 N1 1.9121(13) 3_665 ?
Fe1 N1 1.9122(13) 31_656 ?
Fe1 N1 1.9122(13) 33_546 ?
Fe2 N2 1.9752(13) 3_665 ?
Fe2 N2 1.9752(13) . ?
Fe2 N2 1.9752(13) 33_545 ?
Fe2 N2 1.9752(13) 31_655 ?
Fe2 N2 1.9752(13) 32 ?
Fe2 N2 1.9753(13) 2_655 ?
N1 N4 1.3115(19) . ?
N1 N2 1.3204(19) . ?
N2 N3 1.3327(18) . ?
C1 C2 1.360(4) 24 ?
C1 C2 1.360(4) . ?
C1 C3 1.368(5) 24 ?
C1 C3 1.368(5) . ?
C1 C4 1.472(2) . ?
C2 C3 1.384(4) 12_556 ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 N4 1.328(2) . ?
C4 N3 1.340(2) . ?
N4 H4N 0.8600 . ?
N3 H3N 0.8600 . ?
 
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 32_556 2_655 ?
N1 Fe1 N1 89.70(5) 32_556 . ?
N1 Fe1 N1 90.30(5) 2_655 . ?
N1 Fe1 N1 89.70(5) 32_556 3_665 ?
N1 Fe1 N1 90.30(5) 2_655 3_665 ?
N1 Fe1 N1 90.30(5) . 3_665 ?
N1 Fe1 N1 90.30(5) 32_556 31_656 ?
N1 Fe1 N1 89.70(5) 2_655 31_656 ?
N1 Fe1 N1 180.0 . 31_656 ?
N1 Fe1 N1 89.70(5) 3_665 31_656 ?
N1 Fe1 N1 90.30(5) 32_556 33_546 ?
N1 Fe1 N1 89.70(5) 2_655 33_546 ?
N1 Fe1 N1 89.70(5) . 33_546 ?
N1 Fe1 N1 180.0 3_665 33_546 ?
N1 Fe1 N1 90.29(5) 31_656 33_546 ?
N2 Fe2 N2 90.89(5) 3_665 . ?
N2 Fe2 N2 180.0 3_665 33_545 ?
N2 Fe2 N2 89.12(5) . 33_545 ?
N2 Fe2 N2 89.11(5) 3_665 31_655 ?
N2 Fe2 N2 180.0 . 31_655 ?
N2 Fe2 N2 90.88(5) 33_545 31_655 ?
N2 Fe2 N2 89.12(5) 3_665 32 ?
N2 Fe2 N2 89.11(5) . 32 ?
N2 Fe2 N2 90.88(5) 33_545 32 ?
N2 Fe2 N2 90.88(5) 31_655 32 ?
N2 Fe2 N2 90.88(5) 3_665 2_655 ?
N2 Fe2 N2 90.89(5) . 2_655 ?
N2 Fe2 N2 89.11(5) 33_545 2_655 ?
N2 Fe2 N2 89.11(5) 31_655 2_655 ?
N2 Fe2 N2 180.0 32 2_655 ?
N4 N1 N2 110.78(13) . . ?
N4 N1 Fe1 121.57(11) . . ?
N2 N1 Fe1 127.65(10) . . ?
N1 N2 N3 109.07(13) . . ?
N1 N2 Fe2 122.04(9) . . ?
N3 N2 Fe2 128.90(11) . . ?
C2 C1 C2 24.2(11) 24 . ?
C2 C1 C3 113.3(4) 24 24 ?
C2 C1 C3 118.1(3) . 24 ?
C2 C1 C3 118.1(3) 24 . ?
C2 C1 C3 113.3(4) . . ?
C3 C1 C3 20.6(17) 24 . ?
C2 C1 C4 119.3(2) 24 . ?
C2 C1 C4 119.3(2) . . ?
C3 C1 C4 122.6(2) 24 . ?
C3 C1 C4 122.6(2) . . ?
C1 C2 C3 122.2(4) . 12_556 ?
C1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 12_556 . ?
C1 C3 C2 119.6(3) . 12_556 ?
C1 C3 H3 120.2 . . ?
C2 C3 H3 120.2 12_556 . ?
N4 C4 N3 112.72(15) . . ?
N4 C4 C1 119.23(17) . . ?
N3 C4 C1 128.05(16) . . ?
N1 N4 C4 103.89(14) . . ?
N1 N4 H4N 128.1 . . ?
C4 N4 H4N 128.1 . . ?
N2 N3 C4 103.54(14) . . ?
N2 N3 H3N 128.2 . . ?
C4 N3 H3N 128.2 . . ?
 
_refine_diff_density_max    0.481
_refine_diff_density_min   -0.450
_refine_diff_density_rms    0.050



