#------------------------------------------------------------------------------
#$Date: 2019-11-23 01:08:39 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231731 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/63/4346333.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4346333
loop_
_publ_author_name
'Myers, Thomas W.'
'Chavez, David E.'
'Hanson, Susan K.'
'Scharff, R. Jason'
'Scott, Brian L.'
'Veauthier, Jacqueline M.'
'Wu, Ruilian'
_publ_section_title
;
 Independent Control of Optical and Explosive Properties:
 Pyrazole-Tetrazine Complexes of First Row Transition Metals.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8077
_journal_page_last               8086
_journal_paper_doi               10.1021/acs.inorgchem.5b01313
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C30 H27 B2 F8 Fe N25'
_chemical_formula_weight         967.23
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4405(18)
_cell_length_b                   16.4405(18)
_cell_length_c                   16.4405(18)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.84
_cell_volume                     4443.7(8)
_computing_cell_refinement       'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_collection       'bruker apex'
_computing_data_reduction        'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43069
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.269
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2703
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0954
_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)+(0.0443P)²+29.4686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2193
_refine_ls_wR_factor_ref         0.2219
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2535
_reflns_number_total             2703
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01313_si_002.cif
_cod_data_source_block           TWM3
_cod_original_cell_volume        4443.7(15)
_cod_database_code               4346333
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.938
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'z, x, y'
'-z+1/2, -x, y+1/2'
'z+1/2, -x+1/2, -y'
'-z, x+1/2, -y+1/2'
'y, z, x'
'y+1/2, -z+1/2, -x'
'-y, z+1/2, -x+1/2'
'-y+1/2, -z, x+1/2'
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 0.03491(8) -0.03491(8) -0.53491(8) 0.0232(5) Uani 1 3 d S T P . .
N1 N -0.0396(8) -0.0508(10) -0.2314(6) 0.078(5) Uani 1 1 d . . . . .
H1A H -0.0872 -0.0719 -0.2440 0.094 Uiso 1 1 d R U . . .
H1B H -0.0261 -0.0438 -0.1801 0.094 Uiso 1 1 d R U . . .
N2 N -0.0083(5) -0.0408(6) -0.3668(5) 0.029(2) Uani 1 1 d . . . . .
N3 N 0.0499(5) -0.0253(6) -0.4234(4) 0.027(2) Uani 1 1 d . . . . .
N4 N 0.1411(6) 0.0158(8) -0.3188(6) 0.054(3) Uani 1 1 d . . . . .
N5 N 0.0861(7) 0.0022(10) -0.2643(7) 0.077(5) Uani 1 1 d . . . . .
N6 N 0.1796(5) 0.0062(5) -0.4560(6) 0.035(2) Uani 1 1 d . . . . .
N7 N 0.1542(5) -0.0188(6) -0.5319(6) 0.032(2) Uani 1 1 d . . . . .
C1 C 0.0130(7) -0.0307(13) -0.2895(7) 0.060(4) Uani 1 1 d . . . . .
C2 C 0.1226(7) 0.0004(8) -0.3936(7) 0.038(3) Uani 1 1 d . . . . .
C3 C 0.2173(8) -0.0308(11) -0.6653(7) 0.052(3) Uani 1 1 d . . . . .
H3A H 0.2572 -0.0741 -0.6744 0.079 Uiso 1 1 calc R U . . .
H3B H 0.2316 0.0167 -0.6984 0.079 Uiso 1 1 calc R U . . .
H3C H 0.1631 -0.0501 -0.6807 0.079 Uiso 1 1 calc R U . . .
C4 C 0.2174(7) -0.0089(8) -0.5825(8) 0.042(3) Uani 1 1 d . . . . .
C5 C 0.2840(7) 0.0177(9) -0.5339(9) 0.054(4) Uani 1 1 d . . . . .
H5B H 0.3380 0.0254 -0.5532 0.064 Uiso 1 1 calc R U . . .
C6 C 0.2599(7) 0.0302(9) -0.4571(9) 0.052(3) Uani 1 1 d . . . . .
C7 C 0.3045(7) 0.0620(10) -0.3849(10) 0.062(4) Uani 1 1 d . . . . .
H7A H 0.2806 0.1139 -0.3681 0.093 Uiso 1 1 calc R U . . .
H7B H 0.3619 0.0702 -0.3990 0.093 Uiso 1 1 calc R U . . .
H7C H 0.3005 0.0228 -0.3402 0.093 Uiso 1 1 calc R U . . .
F1 F 0.1590(9) 0.2390(8) -0.3255(8) 0.131(6) Uani 1 1 d . . . . .
F2 F 0.2625(5) 0.2375(5) -0.2375(5) 0.058(4) Uani 1 3 d S T P . .
B1 B 0.2139(10) 0.2861(10) -0.2861(10) 0.074(11) Uani 1 3 d S T P . .
F3 F -0.5306(4) -0.0306(4) -0.4694(4) 0.050(3) Uani 1 3 d S T P . .
F4 F -0.4376(4) -0.0295(4) -0.5714(4) 0.0425(16) Uani 1 1 d . . . . .
B2 B -0.4845(7) 0.0155(7) -0.5155(7) 0.031(5) Uani 1 3 d S T P . .
N8A N 0.3030(12) -0.1970(12) -0.3030(12) 0.141(15) Uani 1 3 d S T P . 1
C8A C 0.199(3) -0.196(3) -0.299(3) 0.111(15) Uiso 0.5 1 d . . P A 1
C9A C 0.164(2) -0.134(2) -0.329(2) 0.076(10) Uiso 0.5 1 d . . P A 1
N8B N 0.0346(19) -0.3161(18) -0.2527(17) 0.120(10) Uiso 0.73(2) 1 d D . P B 2
C8B C 0.073(3) -0.251(3) -0.264(3) 0.151(17) Uiso 0.73(2) 1 d D . P B 2
C9B C 0.101(2) -0.182(2) -0.316(2) 0.116(12) Uiso 0.73(2) 1 d D . P B 2
N8C N 0.095(4) -0.251(4) -0.139(3) 0.10(2) Uiso 0.27(2) 1 d D . P B 3
C8C C 0.091(4) -0.233(5) -0.214(4) 0.08(2) Uiso 0.27(2) 1 d D . P B 3
C9C C 0.164(2) -0.254(3) -0.270(2) 0.031(10) Uiso 0.27(2) 1 d D . P B 3
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'
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
N3 Fe1 N3 93.4(4) . 6_454
N3 Fe1 N3 93.4(4) . 11_554
N3 Fe1 N3 93.4(4) 6_454 11_554
N3 Fe1 N7 80.4(4) . .
N3 Fe1 N7 173.7(4) 6_454 .
N3 Fe1 N7 87.4(4) 11_554 .
N3 Fe1 N7 173.7(4) . 11_554
N3 Fe1 N7 87.4(4) 6_454 11_554
N3 Fe1 N7 80.4(4) 11_554 11_554
N7 Fe1 N7 98.9(4) . 11_554
N3 Fe1 N7 87.4(4) . 6_454
N3 Fe1 N7 80.4(4) 6_454 6_454
N3 Fe1 N7 173.7(4) 11_554 6_454
N7 Fe1 N7 98.9(4) . 6_454
N7 Fe1 N7 98.9(4) 11_554 6_454
C1 N1 H1A 120.4 . .
C1 N1 H1B 119.5 . .
H1A N1 H1B 120.1 . .
C1 N2 N3 116.5(8) . .
N2 N3 C2 115.5(8) . .
N2 N3 Fe1 124.6(6) . .
C2 N3 Fe1 120.0(7) . .
C2 N4 N5 117.4(10) . .
N4 N5 C1 117.9(10) . .
N7 N6 C6 111.4(9) . .
N7 N6 C2 116.2(9) . .
C6 N6 C2 132.3(11) . .
C4 N7 N6 106.9(9) . .
C4 N7 Fe1 140.2(9) . .
N6 N7 Fe1 111.3(6) . .
N2 C1 N1 119.0(11) . .
N2 C1 N5 124.5(10) . .
N1 C1 N5 116.5(12) . .
N4 C2 N3 127.7(10) . .
N4 C2 N6 121.9(11) . .
N3 C2 N6 110.3(10) . .
C4 C3 H3A 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C4 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N7 C4 C3 124.6(12) . .
N7 C4 C5 106.5(11) . .
C3 C4 C5 128.5(11) . .
C6 C5 C4 110.4(10) . .
C6 C5 H5B 124.8 . .
C4 C5 H5B 124.8 . .
C5 C6 N6 104.6(11) . .
C5 C6 C7 131.2(11) . .
N6 C6 C7 124.2(12) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
F1 B1 F1 109.7(13) 7 12_554
F1 B1 F1 109.7(13) 7 .
F1 B1 F1 109.7(13) 12_554 .
F1 B1 F2 109.3(13) 7 .
F1 B1 F2 109.3(13) 12_554 .
F1 B1 F2 109.3(13) . .
F3 B2 F4 112.8(8) . .
F3 B2 F4 112.8(8) . 8_454
F4 B2 F4 105.9(9) . 8_454
F3 B2 F4 112.8(8) . 10_444
F4 B2 F4 105.9(9) . 10_444
F4 B2 F4 105.9(9) 8_454 10_444
C8A N8A C8A 88(3) . 8_544
C8A N8A C8A 88(3) . 10_545
C8A N8A C8A 88(3) 8_544 10_545
C9A C8A N8A 117(4) . .
N8B C8B C9B 153(5) . .
N8C C8C C9C 120(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N3 1.857(8) .
Fe1 N3 1.857(8) 6_454
Fe1 N3 1.857(8) 11_554
Fe1 N7 1.979(8) .
Fe1 N7 1.979(8) 11_554
Fe1 N7 1.979(8) 6_454
N1 C1 1.330(15) .
N1 H1A 0.8809 .
N1 H1B 0.8795 .
N2 C1 1.328(15) .
N2 N3 1.359(10) .
N3 C2 1.359(14) .
N4 C2 1.292(15) .
N4 N5 1.293(15) .
N5 C1 1.381(17) .
N6 N7 1.378(14) .
N6 C6 1.378(14) .
N6 C2 1.394(14) .
N7 C4 1.343(14) .
C3 C4 1.407(18) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.425(18) .
C5 C6 1.34(2) .
C5 H5B 0.9500 .
C6 C7 1.49(2) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
F1 B1 1.354(14) .
F2 B1 1.39(3) .
B1 F1 1.354(14) 7
B1 F1 1.354(14) 12_554
F3 B2 1.31(2) .
F4 B2 1.409(10) .
B2 F4 1.409(10) 8_454
B2 F4 1.409(10) 10_444
N8A C8A 1.71(6) .
N8A C8A 1.71(6) 8_544
N8A C8A 1.71(6) 10_545
C8A C9A 1.27(6) .
N8B C8B 1.25(3) .
C8B C9B 1.50(3) .
N8C C8C 1.26(4) .
C8C C9C 1.55(4) .
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
C1 N2 N3 C2 -1.4(17) .
C1 N2 N3 Fe1 -179.9(12) .
N3 Fe1 N3 N2 9.3(10) 6_454
N3 Fe1 N3 N2 102.8(7) 11_554
N7 Fe1 N3 N2 -170.4(9) .
N7 Fe1 N3 N2 -70.9(9) 6_454
N3 Fe1 N3 C2 -169.2(9) 6_454
N3 Fe1 N3 C2 -75.7(11) 11_554
N7 Fe1 N3 C2 11.1(9) .
N7 Fe1 N3 C2 110.6(9) 6_454
C2 N4 N5 C1 2(2) .
C6 N6 N7 C4 -1.6(13) .
C2 N6 N7 C4 -179.6(10) .
C6 N6 N7 Fe1 -170.1(9) .
C2 N6 N7 Fe1 11.9(11) .
N3 N2 C1 N1 -175.0(15) .
N3 N2 C1 N5 7(3) .
N4 N5 C1 N2 -8(3) .
N4 N5 C1 N1 174.2(16) .
N5 N4 C2 N3 3(2) .
N5 N4 C2 N6 -174.3(13) .
N2 N3 C2 N4 -4.0(19) .
Fe1 N3 C2 N4 174.6(12) .
N2 N3 C2 N6 173.9(9) .
Fe1 N3 C2 N6 -7.4(14) .
N7 N6 C2 N4 174.4(12) .
C6 N6 C2 N4 -3(2) .
N7 N6 C2 N3 -3.6(14) .
C6 N6 C2 N3 178.9(12) .
N6 N7 C4 C3 177.2(13) .
Fe1 N7 C4 C3 -20(2) .
N6 N7 C4 C5 3.9(13) .
Fe1 N7 C4 C5 167.1(10) .
N7 C4 C5 C6 -5.1(17) .
C3 C4 C5 C6 -178.0(15) .
C4 C5 C6 N6 4.0(17) .
C4 C5 C6 C7 -176.2(16) .
N7 N6 C6 C5 -1.6(16) .
C2 N6 C6 C5 176.0(13) .
N7 N6 C6 C7 178.6(13) .
C2 N6 C6 C7 -4(2) .
C8A N8A C8A C9A -152(5) 8_544
C8A N8A C8A C9A 120(6) 10_545
