#------------------------------------------------------------------------------
#$Date: 2025-07-05 09:59:34 +0200 (Sat 05 de Jul de 2025) $
#$Revision: 300364 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/90/7719025.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_7719025
loop_
_publ_author_name
'Benz, Maximilian'
'Endraß, Simon M J'
'Klapötke, Thomas M'
'Stierstorfer, Jörg'
'Strey, Sadiq'
_publ_section_title
;
 1-Amino-5-nitriminotetrazolate as a promising anion in safe yet powerful
 energetic coordination compounds.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6156
_journal_page_last               6166
_journal_paper_doi               10.1039/d4dt03086a
_journal_volume                  54
_journal_year                    2025
_chemical_compound_source
'diaqua bis(1-amino-5-nitriminotetrazolato) iron(II) dihydrate'
_chemical_formula_moiety         'C2 H8 Fe N14 O6, 2(H2 O)'
_chemical_formula_sum            'C2 H12 Fe N14 O8'
_chemical_formula_weight         416.11
_chemical_name_systematic
'diaqua bis(1-amino-5-nitriminotetrazolato) iron(II) dihydrate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-29 deposited with the CCDC.	2025-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                74.463(2)
_cell_angle_beta                 71.796(2)
_cell_angle_gamma                86.373(2)
_cell_formula_units_Z            1
_cell_length_a                   6.4691(4)
_cell_length_b                   6.9872(4)
_cell_length_c                   8.3330(5)
_cell_measurement_reflns_used    6159
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      3.03
_cell_volume                     344.65(4)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_molecular_graphics    'Diamond 2.1c, Crystal Impact GbR'
_computing_publication_material  'Encifer 1.5.1, CCDC 2014'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8421
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.592
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'rotating anode generator'
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.6947
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0245
_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)+(0.0168P)²+0.1948P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1836
_reflns_number_total             1924
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03086a2.cif
_cod_data_source_block           cv065
_cod_database_code               7719025
_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.
;
_olex2_submission_original_sample_id cv065
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 1.000000 0.500000 0.000000 0.01223(8) Uani 1 2 d S . P . .
O4 O 0.42055(17) 0.21479(16) 0.26553(13) 0.0179(2) Uani 1 1 d . . . . .
O3 O 0.72684(17) 0.39220(16) -0.02795(14) 0.0169(2) Uani 1 1 d . . . . .
O2 O 0.67142(18) 0.85644(15) 0.34755(14) 0.0205(2) Uani 1 1 d . . . . .
O1 O 0.7524(2) 0.90277(17) 0.06638(15) 0.0335(3) Uani 1 1 d . . . . .
N1 N 0.87818(18) 0.30216(16) 0.38351(14) 0.0124(2) Uani 1 1 d . . . . .
N7 N 0.74022(19) 0.79527(17) 0.21282(15) 0.0168(2) Uani 1 1 d . . . . .
N5 N 0.98399(19) 0.23819(17) 0.23318(14) 0.0136(2) Uani 1 1 d . . . . .
N4 N 0.72450(18) 0.49859(17) 0.54582(14) 0.0146(2) Uani 1 1 d . . . . .
N6 N 0.80670(18) 0.60791(16) 0.22057(14) 0.0135(2) Uani 1 1 d . . . . .
N2 N 0.85880(19) 0.19893(17) 0.54979(14) 0.0159(2) Uani 1 1 d . . . . .
N3 N 0.76641(19) 0.31794(17) 0.64433(14) 0.0164(2) Uani 1 1 d . . . . .
C1 C 0.79652(19) 0.48608(18) 0.38170(16) 0.0118(2) Uani 1 1 d . . . . .
H5A H 0.909(3) 0.137(3) 0.241(3) 0.025(5) Uiso 1 1 d . . . . .
H5B H 1.111(3) 0.208(3) 0.240(2) 0.022(5) Uiso 1 1 d . . . . .
H4A H 0.460(4) 0.114(4) 0.303(3) 0.037(6) Uiso 1 1 d . . . . .
H4B H 0.388(4) 0.269(3) 0.338(3) 0.033(6) Uiso 1 1 d . . . . .
H3A H 0.628(4) 0.347(3) 0.052(3) 0.029(5) Uiso 1 1 d . . . . .
H3B H 0.736(4) 0.342(3) -0.099(3) 0.039(6) Uiso 1 1 d . . . . .
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O3 Fe1 O3 180.0 . 2_765 ?
O3 Fe1 N5 90.31(4) . . ?
O3 Fe1 N5 89.69(4) 2_765 . ?
O3 Fe1 N5 89.69(4) . 2_765 ?
O3 Fe1 N5 90.31(4) 2_765 2_765 ?
O3 Fe1 N6 91.95(4) . . ?
O3 Fe1 N6 88.05(4) . 2_765 ?
O3 Fe1 N6 91.95(4) 2_765 2_765 ?
O3 Fe1 N6 88.05(4) 2_765 . ?
N5 Fe1 N5 180.0 2_765 . ?
N6 Fe1 N5 103.37(4) 2_765 . ?
N6 Fe1 N5 103.37(4) . 2_765 ?
N6 Fe1 N5 76.63(4) . . ?
N6 Fe1 N5 76.63(4) 2_765 2_765 ?
N6 Fe1 N6 180.0 . 2_765 ?
H4A O4 H4B 108(2) . . ?
Fe1 O3 H3A 121.8(15) . . ?
Fe1 O3 H3B 121.0(18) . . ?
H3A O3 H3B 109(2) . . ?
N2 N1 N5 125.75(10) . . ?
N2 N1 C1 109.65(10) . . ?
C1 N1 N5 124.36(10) . . ?
O2 N7 N6 121.40(11) . . ?
O1 N7 O2 122.18(12) . . ?
O1 N7 N6 116.42(11) . . ?
Fe1 N5 H5A 115.4(13) . . ?
Fe1 N5 H5B 110.5(13) . . ?
N1 N5 Fe1 106.98(7) . . ?
N1 N5 H5A 105.3(13) . . ?
N1 N5 H5B 104.9(13) . . ?
H5A N5 H5B 112.9(18) . . ?
C1 N4 N3 105.24(10) . . ?
N7 N6 Fe1 125.54(8) . . ?
N7 N6 C1 117.51(11) . . ?
C1 N6 Fe1 115.20(8) . . ?
N3 N2 N1 105.12(10) . . ?
N2 N3 N4 112.37(10) . . ?
N1 C1 N6 115.95(11) . . ?
N4 C1 N1 107.62(11) . . ?
N4 C1 N6 136.43(12) . . ?
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 O3 2.0649(10) . ?
Fe1 O3 2.0649(10) 2_765 ?
Fe1 N5 2.2642(11) . ?
Fe1 N5 2.2642(11) 2_765 ?
Fe1 N6 2.1674(11) . ?
Fe1 N6 2.1674(11) 2_765 ?
O4 H4A 0.76(3) . ?
O4 H4B 0.77(2) . ?
O3 H3A 0.77(2) . ?
O3 H3B 0.75(2) . ?
O2 N7 1.2498(15) . ?
O1 N7 1.2313(16) . ?
N1 N5 1.4011(15) . ?
N1 N2 1.3503(15) . ?
N1 C1 1.3563(16) . ?
N7 N6 1.3430(15) . ?
N5 H5A 0.86(2) . ?
N5 H5B 0.85(2) . ?
N4 N3 1.3716(16) . ?
N4 C1 1.3251(16) . ?
N6 C1 1.3680(16) . ?
N2 N3 1.2897(16) . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4B N4 0.77(2) 2.09(2) 2.8088(16) 157(2) 2_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
Fe1 N6 C1 N1 -10.05(14) . . . . ?
Fe1 N6 C1 N4 170.12(12) . . . . ?
O2 N7 N6 Fe1 -164.17(9) . . . . ?
O2 N7 N6 C1 -0.05(18) . . . . ?
O1 N7 N6 Fe1 15.34(18) . . . . ?
O1 N7 N6 C1 179.46(12) . . . . ?
N1 N2 N3 N4 -0.36(14) . . . . ?
N7 N6 C1 N1 -175.80(11) . . . . ?
N7 N6 C1 N4 4.4(2) . . . . ?
N5 N1 N2 N3 175.03(11) . . . . ?
N5 N1 C1 N4 -175.08(11) . . . . ?
N5 N1 C1 N6 5.04(18) . . . . ?
N2 N1 N5 Fe1 -171.50(10) . . . . ?
N2 N1 C1 N4 -0.45(14) . . . . ?
N2 N1 C1 N6 179.67(10) . . . . ?
N3 N4 C1 N1 0.22(13) . . . . ?
N3 N4 C1 N6 -179.94(14) . . . . ?
C1 N1 N5 Fe1 2.26(14) . . . . ?
C1 N1 N2 N3 0.50(14) . . . . ?
C1 N4 N3 N2 0.09(14) . . . . ?
