Synthesis and characterization of cyclo-pentazolate salts of iron(iii) and aluminum(iii)
Chen, Lei; Yang, Chen; Hu, Haoran; Shi, Lei; Zhang, Chong; Sun, Chengguo; Gao, Chao; Du, Yang; Hu, Bingcheng; CrystEngComm  (2022) –; doi:10.1039/D2CE01270G

data_7245781
_publ_section_title
;
 Synthesis and characterization of cyclo-pentazolate salts of iron(iii)
 and aluminum(iii)
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01270G
_journal_year                    2022
_chemical_formula_moiety         'Fe H12 O6, 9(H2 O), 3(N5)'
_chemical_formula_sum            'Fe H30 N15 O15'
_chemical_formula_weight         536.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8316(4)
_cell_length_b                   14.7115(4)
_cell_length_c                   20.1791(6)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.455
_cell_measurement_theta_min      2.680
_cell_volume                     4987.9(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56395
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.065
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.9328.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         11374
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.9100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6673
_reflns_number_total             11374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01270g2.cif
_cod_data_source_block           mo_20220304_cl_fe_0m
_cod_database_code               7245781
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Fe2-H11A \\sim Fe2-H11B
 with sigma of 0.02
 Fe2-H10A \\sim Fe2-H10B
 with sigma of 0.02
 Fe2-H9A \\sim Fe2-H9B
 with sigma of 0.02
 Fe1-H1A \\sim Fe1-H1B
 with sigma of 0.02
 Fe1-H5A \\sim Fe1-H5B
 with sigma of 0.02
 Fe1-H2A \\sim Fe1-H2B
 with sigma of 0.02
 Fe2-H8A \\sim Fe2-H8B
 with sigma of 0.02
 Fe2-H12A \\sim Fe2-H12B
 with sigma of 0.02
 Fe1-H4A \\sim Fe1-H4B
 with sigma of 0.02
 Fe1-H6A \\sim Fe1-H6B
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B), O8(H8A,H8B),
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B),
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B),
  O19(H19A,H19B), O20(H20A,H20B), O21(H21A,H21B), O22(H22A,H22B), O23(H23A,
 H23B), O24(H24A,H24B), O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B),
 O28(H28A,H28B), O29(H29A,H29B), O30(H30A,H30B)
3.b Rotating group:
 O3(H3A,H3B), O7(H7A,H7B)
;
_shelx_res_checksum              97648
_shelx_hkl_checksum              10462
_olex2_submission_special_instructions 'No special instructions were received'