 
data_Fe_tetrazol_RT_0ma_a
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C12 H6 Fe N12, 3(H2 O)'
_chemical_formula_sum
 'C12 H12 Fe N12 O3' 
_chemical_formula_weight          428.14

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0192   0.0096
 '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'  -1.0935   3.1934
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0330   0.0189
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0517   0.0336
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            148
_space_group_name_H-M_alt         'R -3 :H'
_space_group_name_Hall            '-R 3'
 
_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'
 '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'
 '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'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -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'
 '-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'
 
_cell_length_a                    22.5930(7)
_cell_length_b                    22.5930(7)
_cell_length_c                    7.4636(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      3299.3(2)
_cell_formula_units_Z             6
_cell_measurement_temperature     299(2)
_cell_measurement_reflns_used      9280
_cell_measurement_theta_min        6.35
_cell_measurement_theta_max       72.35
 
_exptl_crystal_description        hexagonal
_exptl_crystal_colour             orange
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.275          
_exptl_crystal_F_000              1272
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     5.821
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'numerical'
_exptl_absorpt_correction_T_min   0.500
_exptl_absorpt_correction_T_max   0.900
_exptl_absorpt_process_details    'SADABS'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       299(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             16951
_diffrn_reflns_av_unetI/netI      0.0194
_diffrn_reflns_av_R_equivalents   0.0430
_diffrn_reflns_limit_h_min        -27
_diffrn_reflns_limit_h_max        27
_diffrn_reflns_limit_k_min        -27
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          10.402
_diffrn_reflns_theta_max          72.347
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.589
_diffrn_measured_fraction_theta_full  0.567
_diffrn_reflns_Laue_measured_fraction_max    0.589
_diffrn_reflns_Laue_measured_fraction_full   0.567
_diffrn_reflns_point_group_measured_fraction_max   0.589
_diffrn_reflns_point_group_measured_fraction_full  0.567
_reflns_number_total              862
_reflns_number_gt                 841
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.1795P)²+28.8481P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0030(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          862
_refine_ls_number_parameters      132
_refine_ls_number_restraints      72
_refine_ls_R_factor_all           0.0985
_refine_ls_R_factor_gt            0.0972
_refine_ls_wR_factor_ref          0.2661
_refine_ls_wR_factor_gt           0.2642
_refine_ls_goodness_of_fit_ref    1.075
_refine_ls_restrained_S_all       1.113
_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 0.6667 0.3333 0.3333 0.0113(8) Uani 1 6 d S T P . .
Fe2 Fe 0.6667 0.3333 0.8333 0.0134(8) Uani 1 6 d S T P . .
C1 C 0.5727(4) 0.4269(4) 0.5472(10) 0.0354(15) Uani 1 1 d . U . . .
C2 C 0.5352(4) 0.4648(4) 0.5250(10) 0.0436(18) Uani 1 1 d . U . . .
C3 C 0.4776(10) 0.4492(10) 0.639(2) 0.037(3) Uani 0.4 1 d . U P A 1
H3 H 0.4628 0.4150 0.7251 0.044 Uiso 0.4 1 calc R U P A 1
C4 C 0.5552(10) 0.5126(10) 0.385(2) 0.038(3) Uani 0.4 1 d . U P A 1
H4 H 0.5902 0.5189 0.3075 0.045 Uiso 0.4 1 calc R U P A 1
N1 N 0.6251(2) 0.3755(2) 0.4805(6) 0.0191(11) Uani 1 1 d . . . . .
N2 N 0.6226(3) 0.3777(3) 0.6553(7) 0.0245(12) Uani 1 1 d . U . . .
N3 N 0.5944(2) 0.4064(2) 0.4077(6) 0.0247(12) Uani 1 1 d . U . . .
N4 N 0.5895(3) 0.4103(3) 0.7013(8) 0.0426(16) Uani 1 1 d . . . . .
C3A C 0.5459(9) 0.5177(10) 0.640(2) 0.037(3) Uani 0.4 1 d . U P A 2
H3A H 0.5753 0.5279 0.7366 0.045 Uiso 0.4 1 calc R U P A 2
C4A C 0.4857(10) 0.4445(10) 0.386(2) 0.039(3) Uani 0.4 1 d . U P A 2
H4A H 0.4750 0.4067 0.3143 0.047 Uiso 0.4 1 calc R U P A 2
C3B C 0.510(2) 0.478(2) 0.648(4) 0.032(6) Uani 0.2 1 d . U P A 3
H3B H 0.5093 0.4590 0.7583 0.038 Uiso 0.2 1 calc R U P A 3
C4B C 0.518(2) 0.477(2) 0.363(5) 0.035(6) Uani 0.2 1 d . U P A 3
H4B H 0.5248 0.4575 0.2601 0.042 Uiso 0.2 1 calc R U P A 3
O1W O 0.7485(16) 0.5432(9) 0.612(3) 0.113(8) Uani 0.6 1 d . U P B 1
O2W O 0.7959(17) 0.5426(12) 0.614(3) 0.093(9) Uani 0.4 1 d . U P C 2
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Fe1 N1 1.973(4) 3_665 ?
Fe1 N1 1.973(4) 2_655 ?
Fe1 N1 1.973(4) . ?
Fe1 N1 1.973(4) 16_655 ?
Fe1 N1 1.973(4) 18_545 ?
Fe1 N1 1.973(4) 17 ?
Fe2 N2 2.181(5) 16_656 ?
Fe2 N2 2.181(5) 17_556 ?
Fe2 N2 2.181(5) 18_546 ?
Fe2 N2 2.181(5) 2_655 ?
Fe2 N2 2.181(5) 3_665 ?
Fe2 N2 2.181(5) . ?
C1 N4 1.323(10) . ?
C1 N3 1.329(8) . ?
C1 C2 1.484(9) . ?
C2 C3B 1.19(3) . ?
C2 C4B 1.34(4) . ?
C2 C3A 1.391(19) . ?
C2 C4 1.408(19) . ?
C2 C4A 1.425(19) . ?
C2 C3 1.44(2) . ?
C3 C4 1.40(2) 10_666 ?
C3 H3 0.9300 . ?
C4 C3 1.40(2) 10_666 ?
C4 H4 0.9300 . ?
N1 N2 1.308(7) . ?
N1 N3 1.322(6) . ?
N2 N4 1.330(7) . ?
C3A C4A 1.37(2) 10_666 ?
C3A H3A 0.9300 . ?
C4A C3A 1.37(2) 10_666 ?
C4A H4A 0.9300 . ?
C3B C4B 1.44(4) 10_666 ?
C3B H3B 0.9300 . ?
C4B C3B 1.44(4) 10_666 ?
C4B H4B 0.9300 . ?
 
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 91.99(16) 3_665 2_655 ?
N1 Fe1 N1 92.00(16) 3_665 . ?
N1 Fe1 N1 91.99(16) 2_655 . ?
N1 Fe1 N1 88.01(16) 3_665 16_655 ?
N1 Fe1 N1 88.01(16) 2_655 16_655 ?
N1 Fe1 N1 180.0(2) . 16_655 ?
N1 Fe1 N1 180.0 3_665 18_545 ?
N1 Fe1 N1 88.01(16) 2_655 18_545 ?
N1 Fe1 N1 88.00(16) . 18_545 ?
N1 Fe1 N1 92.00(16) 16_655 18_545 ?
N1 Fe1 N1 88.01(16) 3_665 17 ?
N1 Fe1 N1 180.0 2_655 17 ?
N1 Fe1 N1 88.00(16) . 17 ?
N1 Fe1 N1 92.00(16) 16_655 17 ?
N1 Fe1 N1 92.00(16) 18_545 17 ?
N2 Fe2 N2 86.77(19) 16_656 17_556 ?
N2 Fe2 N2 86.77(19) 16_656 18_546 ?
N2 Fe2 N2 86.77(19) 17_556 18_546 ?
N2 Fe2 N2 93.23(19) 16_656 2_655 ?
N2 Fe2 N2 180.0 17_556 2_655 ?
N2 Fe2 N2 93.23(19) 18_546 2_655 ?
N2 Fe2 N2 93.23(19) 16_656 3_665 ?
N2 Fe2 N2 93.23(19) 17_556 3_665 ?
N2 Fe2 N2 180.0 18_546 3_665 ?
N2 Fe2 N2 86.77(19) 2_655 3_665 ?
N2 Fe2 N2 180.0(2) 16_656 . ?
N2 Fe2 N2 93.23(19) 17_556 . ?
N2 Fe2 N2 93.23(19) 18_546 . ?
N2 Fe2 N2 86.77(19) 2_655 . ?
N2 Fe2 N2 86.77(19) 3_665 . ?
N4 C1 N3 112.0(6) . . ?
N4 C1 C2 126.0(6) . . ?
N3 C1 C2 122.0(6) . . ?
C3B C2 C4B 115(2) . . ?
C3A C2 C4A 119.7(11) . . ?
C4 C2 C3 121.9(10) . . ?
C3B C2 C1 122.8(17) . . ?
C4B C2 C1 121.6(15) . . ?
C3A C2 C1 121.6(9) . . ?
C4 C2 C1 118.1(9) . . ?
C4A C2 C1 118.6(9) . . ?
C3 C2 C1 119.9(9) . . ?
C4 C3 C2 117.8(15) 10_666 . ?
C4 C3 H3 121.1 10_666 . ?
C2 C3 H3 121.1 . . ?
C3 C4 C2 120.1(15) 10_666 . ?
C3 C4 H4 120.0 10_666 . ?
C2 C4 H4 120.0 . . ?
N2 N1 N3 110.3(4) . . ?
N2 N1 Fe1 127.8(3) . . ?
N3 N1 Fe1 121.9(4) . . ?
N1 N2 N4 108.9(4) . . ?
N1 N2 Fe2 123.5(3) . . ?
N4 N2 Fe2 127.5(4) . . ?
N1 N3 C1 104.1(5) . . ?
C1 N4 N2 104.7(5) . . ?
C4A C3A C2 122.0(16) 10_666 . ?
C4A C3A H3A 119.0 10_666 . ?
C2 C3A H3A 119.0 . . ?
C3A C4A C2 118.1(15) 10_666 . ?
C3A C4A H4A 121.0 10_666 . ?
C2 C4A H4A 121.0 . . ?
C2 C3B C4B 125(3) . 10_666 ?
C2 C3B H3B 117.5 . . ?
C4B C3B H3B 117.5 10_666 . ?
C2 C4B C3B 118(3) . 10_666 ?
C2 C4B H4B 121.1 . . ?
C3B C4B H4B 121.1 10_666 . ?
 
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
N4 C1 C2 C3B -8(3) . . . . ?
N3 C1 C2 C3B 174(3) . . . . ?
N4 C1 C2 C4B -178(2) . . . . ?
N3 C1 C2 C4B 4(3) . . . . ?
N4 C1 C2 C3A 36.9(15) . . . . ?
N3 C1 C2 C3A -141.9(12) . . . . ?
N4 C1 C2 C4 141.8(12) . . . . ?
N3 C1 C2 C4 -37.0(14) . . . . ?
N4 C1 C2 C4A -141.0(12) . . . . ?
N3 C1 C2 C4A 40.2(14) . . . . ?
N4 C1 C2 C3 -41.8(15) . . . . ?
N3 C1 C2 C3 139.4(12) . . . . ?
C4 C2 C3 C4 -5(3) . . . 10_666 ?
C1 C2 C3 C4 178.7(14) . . . 10_666 ?
C3 C2 C4 C3 5(3) . . . 10_666 ?
C1 C2 C4 C3 -178.5(15) . . . 10_666 ?
N3 N1 N2 N4 0.2(7) . . . . ?
Fe1 N1 N2 N4 -179.4(4) . . . . ?
N3 N1 N2 Fe2 -180.0(3) . . . . ?
Fe1 N1 N2 Fe2 0.4(7) . . . . ?
N2 N1 N3 C1 -0.5(6) . . . . ?
Fe1 N1 N3 C1 179.1(4) . . . . ?
N4 C1 N3 N1 0.7(7) . . . . ?
C2 C1 N3 N1 179.6(6) . . . . ?
N3 C1 N4 N2 -0.5(8) . . . . ?
C2 C1 N4 N2 -179.4(7) . . . . ?
N1 N2 N4 C1 0.2(8) . . . . ?
Fe2 N2 N4 C1 -179.6(5) . . . . ?
C4A C2 C3A C4A -6(3) . . . 10_666 ?
C1 C2 C3A C4A 176.3(15) . . . 10_666 ?
C3A C2 C4A C3A 6(3) . . . 10_666 ?
C1 C2 C4A C3A -176.5(14) . . . 10_666 ?
C4B C2 C3B C4B -18(6) . . . 10_666 ?
C1 C2 C3B C4B 171(3) . . . 10_666 ?
C3B C2 C4B C3B 17(6) . . . 10_666 ?
C1 C2 C4B C3B -172(3) . . . 10_666 ?
 
_refine_diff_density_max    0.643
_refine_diff_density_min   -0.408
_refine_diff_density_rms    0.093



