#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:36:09 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223555 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/38/7233849.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_7233849 loop_ _publ_author_name 'Wang, Yanna' 'Yang, Xiaoming' 'Zhang, Weijing' 'Li, Haibo' 'Li, Zhimin' 'Wang, Lin' 'Zhang, Tonglai' _publ_section_title ; Energetic transition metal salts of 5,5′-dinitramino-3,3′-methylene-1H-1,2,4-bistriazole: syntheses, structures and properties ; _journal_issue 42 _journal_name_full CrystEngComm _journal_page_first 6452 _journal_paper_doi 10.1039/C9CE01158G _journal_volume 21 _journal_year 2019 _chemical_formula_moiety 'C5 H10 Fe N10 O9, 4(H2 O)' _chemical_formula_sum 'C5 H18 Fe N10 O13' _chemical_formula_weight 482.14 _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _audit_creation_date 2019-09-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-09-06 deposited with the CCDC. 2019-09-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4366(17) _cell_length_b 9.839(2) _cell_length_c 20.798(4) _cell_measurement_reflns_used 5356 _cell_measurement_temperature 163(2) _cell_measurement_theta_max 27.4739 _cell_measurement_theta_min 2.0699 _cell_volume 1726.4(6) _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)' _diffrn_ambient_temperature 163.15 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type AFC10\SATURN724+ _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0283 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 6354 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.486 _diffrn_reflns_theta_min 3.109 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.855 _exptl_crystal_description block _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.336 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 1975 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0368 _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/[\s^2^(Fo^2^)+(0.0352P)^2^+1.8961P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.0883 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1862 _reflns_number_total 1975 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL bwn18357_pl_a.res in Pccn bwn18357_pl.res created by SHELXL-2018/3 at 15:48:04 on 06-Sep-2019 CELL 0.71073 8.4366 9.8389 20.7983 90 90 90 ZERR 4 0.0017 0.002 0.0042 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H Fe N O UNIT 20 72 4 40 52 L.S. 5 PLAN -5 SIZE 0.21 0.2 0.14 TEMP -110 BOND $H list 4 CONF fmap 2 acta OMIT 2 3 5 OMIT 0 0 2 REM REM REM WGHT 0.035200 1.896100 FVAR 0.33018 FE1 3 0.250000 0.250000 0.399811 10.50000 0.01063 0.01472 = 0.01230 0.00000 0.00000 -0.00118 O5 5 0.159282 0.455788 0.403748 11.00000 0.01258 0.01743 = 0.01637 0.00189 0.00026 -0.00168 AFIX 3 0.8400 H5A 2 0.067812 0.460688 0.419528 11.00000 -1.20000 H5B 2 0.153762 0.488818 0.366578 11.00000 -1.20000 AFIX 0 O4 5 0.099286 0.191305 0.322749 11.00000 0.01526 0.02877 = 0.01533 0.00145 -0.00187 -0.00434 AFIX 3 0.8400 H4A 2 0.074586 0.241985 0.291839 11.00000 -1.20000 H4B 2 0.009516 0.172665 0.337849 11.00000 -1.20000 AFIX 0 O2 5 0.847586 0.459490 0.453448 11.00000 0.01310 0.02224 = 0.01969 -0.00274 -0.00161 -0.00414 O1 5 0.821370 0.437978 0.349586 11.00000 0.02000 0.03575 = 0.01782 0.00045 0.00487 -0.00582 O3 5 0.250000 0.250000 0.634383 10.50000 0.02006 0.03564 = 0.01447 0.00000 0.00000 -0.00617 O7 5 0.835956 0.423938 0.711724 11.00000 0.04586 0.02845 = 0.02129 0.00308 -0.00008 0.00748 AFIX 3 0.8400 H7A 2 0.891936 0.353388 0.713024 11.00000 -1.20000 H7B 2 0.867986 0.480368 0.739104 11.00000 -1.20000 AFIX 0 O6 5 0.506408 0.355990 0.721489 11.00000 0.04739 0.04712 = 0.01576 0.00439 -0.00650 -0.01375 AFIX 3 0.8400 H6A 2 0.601518 0.381300 0.721779 11.00000 -1.20000 H6B 2 0.468708 0.371180 0.684820 11.00000 -1.20000 AFIX 0 N5 4 0.416484 0.298384 0.476010 11.00000 0.01027 0.01348 = 0.01624 -0.00135 -0.00055 -0.00116 N1 4 0.767621 0.423370 0.404491 11.00000 0.01260 0.01645 = 0.01836 -0.00133 0.00062 -0.00022 N3 4 0.622930 0.374007 0.528854 11.00000 0.01111 0.01598 = 0.01737 -0.00105 -0.00096 -0.00264 AFIX 3 0.8500 H3 2 0.705970 0.418417 0.538544 11.00000 -1.20000 AFIX 0 N4 4 0.516127 0.338551 0.575010 11.00000 0.01380 0.01757 = 0.01633 -0.00092 -0.00049 -0.00222 N2 4 0.625065 0.368779 0.409698 11.00000 0.01110 0.02051 = 0.01864 -0.00181 0.00126 -0.00281 C1 1 0.563422 0.350271 0.469775 11.00000 0.01166 0.01096 = 0.01775 -0.00177 -0.00121 0.00140 C2 1 0.394709 0.293911 0.541042 11.00000 0.01288 0.01280 = 0.01595 -0.00079 -0.00145 0.00015 C3 1 0.250000 0.250000 0.576038 10.50000 0.01523 0.01514 = 0.01631 0.00000 0.00000 -0.00110 HKLF 4 REM bwn18357_pl_a.res in Pccn REM wR2 = 0.0883, GooF = S = 1.103, Restrained GooF = 1.103 for all data REM R1 = 0.0368 for 1862 Fo > 4sig(Fo) and 0.0395 for all 1975 data REM 133 parameters refined using 0 restraints END WGHT 0.0352 1.8962 REM Highest difference peak 0.336, deepest hole -0.336, 1-sigma level 0.073 Q1 1 0.1472 0.2048 0.4557 11.00000 0.05 0.34 Q2 1 0.1684 0.2350 0.5582 11.00000 0.05 0.26 Q3 1 0.3973 0.2961 0.5084 11.00000 0.05 0.26 Q4 1 0.1416 0.1017 0.2798 11.00000 0.05 0.24 Q5 1 0.4875 0.3016 0.6771 11.00000 0.05 0.23 REM The information below was added by Olex2. REM REM R1 = 0.0368 for 1862 Fo > 4sig(Fo) and 0.0395 for all 6978 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.34, deepest hole -0.34 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0395 REM R1_gt = 0.0368 REM wR_ref = 0.0883 REM GOOF = 1.103 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 6978 REM Reflections_gt = 1862 REM Parameters = n/a REM Hole = -0.34 REM Peak = 0.34 REM Flack = n/a ; _cod_data_source_file c9ce01158g2.cif _cod_data_source_block bwn18357_pl _cod_depositor_comments 'Adding full bibliography for 7233844--7233849.cif.' _cod_database_code 7233849 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.876 _shelx_estimated_absorpt_t_min 0.823 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All N(H) groups, All O(H,H) groups 2.a Riding coordinates: O5(H5A,H5B), O4(H4A,H4B), O7(H7A,H7B), O6(H6A,H6B), N3(H3) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-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 Fe1 Fe 0.250000 0.250000 0.39981(2) 0.01255(13) Uani 1 2 d S T P O5 O 0.15928(16) 0.45579(14) 0.40375(6) 0.0155(3) Uani 1 1 d . . . H5A H 0.067812 0.460688 0.419528 0.019 Uiso 1 1 d R . . H5B H 0.153762 0.488818 0.366578 0.019 Uiso 1 1 d R . . O4 O 0.09929(16) 0.19130(15) 0.32275(7) 0.0198(3) Uani 1 1 d . . . H4A H 0.074586 0.241985 0.291839 0.024 Uiso 1 1 d R . . H4B H 0.009516 0.172665 0.337849 0.024 Uiso 1 1 d R . . O2 O 0.84759(16) 0.45949(14) 0.45345(7) 0.0183(3) Uani 1 1 d . . . O1 O 0.82137(18) 0.43798(17) 0.34959(7) 0.0245(4) Uani 1 1 d . . . O3 O 0.250000 0.250000 0.63438(10) 0.0234(5) Uani 1 2 d S T P O7 O 0.8360(2) 0.42394(17) 0.71172(8) 0.0319(4) Uani 1 1 d . . . H7A H 0.891936 0.353388 0.713024 0.038 Uiso 1 1 d R . . H7B H 0.867986 0.480368 0.739104 0.038 Uiso 1 1 d R . . O6 O 0.5064(2) 0.35599(19) 0.72149(8) 0.0368(4) Uani 1 1 d . . . H6A H 0.601518 0.381300 0.721779 0.044 Uiso 1 1 d R . . H6B H 0.468708 0.371180 0.684820 0.044 Uiso 1 1 d R . . N5 N 0.41648(18) 0.29838(16) 0.47601(8) 0.0133(3) Uani 1 1 d . . . N1 N 0.7676(2) 0.42337(18) 0.40449(8) 0.0158(3) Uani 1 1 d . . . N3 N 0.62293(19) 0.37401(17) 0.52885(8) 0.0148(3) Uani 1 1 d . . . H3 H 0.705970 0.418417 0.538544 0.018 Uiso 1 1 d R . . N4 N 0.51613(19) 0.33855(16) 0.57501(8) 0.0159(3) Uani 1 1 d . . . N2 N 0.62506(19) 0.36878(18) 0.40970(8) 0.0168(3) Uani 1 1 d . . . C1 C 0.5634(2) 0.35027(18) 0.46977(9) 0.0135(4) Uani 1 1 d . . . C2 C 0.3947(2) 0.29391(19) 0.54104(9) 0.0139(4) Uani 1 1 d . . . C3 C 0.250000 0.250000 0.57604(13) 0.0156(5) Uani 1 2 d S T P 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 0.0106(2) 0.0147(2) 0.0123(2) 0.000 0.000 -0.00118(14) O5 0.0126(7) 0.0174(7) 0.0164(7) 0.0019(5) 0.0003(5) -0.0017(5) O4 0.0153(7) 0.0288(8) 0.0153(7) 0.0014(6) -0.0019(6) -0.0043(6) O2 0.0131(6) 0.0222(7) 0.0197(7) -0.0027(6) -0.0016(5) -0.0041(5) O1 0.0200(8) 0.0358(9) 0.0178(7) 0.0004(6) 0.0049(6) -0.0058(7) O3 0.0201(11) 0.0356(13) 0.0145(9) 0.000 0.000 -0.0062(9) O7 0.0459(11) 0.0285(8) 0.0213(8) 0.0031(7) -0.0001(7) 0.0075(8) O6 0.0474(11) 0.0471(11) 0.0158(7) 0.0044(7) -0.0065(7) -0.0138(9) N5 0.0103(7) 0.0135(7) 0.0162(8) -0.0014(6) -0.0006(6) -0.0012(6) N1 0.0126(8) 0.0164(8) 0.0184(8) -0.0013(6) 0.0006(6) -0.0002(6) N3 0.0111(7) 0.0160(8) 0.0174(8) -0.0011(6) -0.0010(6) -0.0026(6) N4 0.0138(8) 0.0176(8) 0.0163(8) -0.0009(6) -0.0005(6) -0.0022(6) N2 0.0111(8) 0.0205(8) 0.0186(8) -0.0018(7) 0.0013(6) -0.0028(7) C1 0.0117(8) 0.0110(8) 0.0177(9) -0.0018(7) -0.0012(7) 0.0014(7) C2 0.0129(8) 0.0128(8) 0.0160(9) -0.0008(7) -0.0014(7) 0.0001(7) C3 0.0152(13) 0.0151(12) 0.0163(13) 0.000 0.000 -0.0011(10) 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 O5 Fe1 O5 175.67(7) 2 . O5 Fe1 N5 87.06(6) 2 . O5 Fe1 N5 87.06(6) . 2 O5 Fe1 N5 89.77(6) . . O5 Fe1 N5 89.77(6) 2 2 O4 Fe1 O5 94.08(5) . . O4 Fe1 O5 89.19(5) 2 . O4 Fe1 O5 89.19(5) . 2 O4 Fe1 O5 94.08(5) 2 2 O4 Fe1 O4 82.13(8) 2 . O4 Fe1 N5 95.96(6) 2 . O4 Fe1 N5 175.67(6) 2 2 O4 Fe1 N5 175.67(6) . . O4 Fe1 N5 95.96(6) . 2 N5 Fe1 N5 86.20(9) . 2 Fe1 O5 H5A 113.1 . . Fe1 O5 H5B 110.3 . . H5A O5 H5B 106.6 . . Fe1 O4 H4A 124.3 . . Fe1 O4 H4B 108.5 . . H4A O4 H4B 101.1 . . H7A O7 H7B 110.1 . . H6A O6 H6B 108.4 . . C1 N5 Fe1 127.48(13) . . C1 N5 C2 103.38(16) . . C2 N5 Fe1 128.98(13) . . O2 N1 N2 122.04(16) . . O1 N1 O2 120.80(17) . . O1 N1 N2 117.16(16) . . N4 N3 H3 120.7 . . C1 N3 H3 127.8 . . C1 N3 N4 110.60(15) . . C2 N4 N3 102.79(16) . . N1 N2 C1 118.41(16) . . N5 C1 N3 108.71(16) . . N5 C1 N2 119.28(17) . . N3 C1 N2 132.01(17) . . N5 C2 C3 127.24(18) . . N4 C2 N5 114.52(17) . . N4 C2 C3 118.19(18) . . O3 C3 C2 119.34(12) . 2 O3 C3 C2 119.34(12) . . C2 C3 C2 121.3(2) 2 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 O5 2.1661(14) . Fe1 O5 2.1661(14) 2 Fe1 O4 2.1258(14) 2 Fe1 O4 2.1258(14) . Fe1 N5 2.1705(16) . Fe1 N5 2.1705(16) 2 O5 H5A 0.8400 . O5 H5B 0.8399 . O4 H4A 0.8399 . O4 H4B 0.8401 . O2 N1 1.272(2) . O1 N1 1.237(2) . O3 C3 1.213(4) . O7 H7A 0.8400 . O7 H7B 0.8400 . O6 H6A 0.8402 . O6 H6B 0.8397 . N5 C1 1.347(2) . N5 C2 1.366(2) . N1 N2 1.322(2) . N3 H3 0.8499 . N3 N4 1.362(2) . N3 C1 1.348(2) . N4 C2 1.320(2) . N2 C1 1.366(3) . C2 C3 1.486(2) . 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_4 Fe1 N5 C1 N3 175.74(12) . Fe1 N5 C1 N2 -4.6(3) . Fe1 N5 C2 N4 -175.58(12) . Fe1 N5 C2 C3 2.0(3) . O2 N1 N2 C1 -0.4(3) . O1 N1 N2 C1 179.39(17) . N5 C2 C3 O3 178.96(14) . N5 C2 C3 C2 -1.04(14) 2 N1 N2 C1 N5 178.12(16) . N1 N2 C1 N3 -2.3(3) . N3 N4 C2 N5 0.0(2) . N3 N4 C2 C3 -177.81(14) . N4 N3 C1 N5 -0.2(2) . N4 N3 C1 N2 -179.80(19) . N4 C2 C3 O3 -3.57(19) . N4 C2 C3 C2 176.43(19) 2 C1 N5 C2 N4 -0.1(2) . C1 N5 C2 C3 177.47(15) . C1 N3 N4 C2 0.1(2) . C2 N5 C1 N3 0.1(2) . C2 N5 C1 N2 179.84(17) .