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_7245782
_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         'Al H12 O6, 9(H2 O), 3(N5)'
_chemical_formula_sum            'Al H30 N15 O15'
_chemical_formula_weight         507.37
_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             2021-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.771(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7321(8)
_cell_length_b                   14.5671(6)
_cell_length_c                   20.0005(7)
_cell_measurement_reflns_used    9325
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.44
_cell_volume                     4869.2(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75466
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         2.088
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0112
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1098 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.4058.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+4.8260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5349
_reflns_number_total             8507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01270g2.cif
_cod_data_source_block           mo_0416_4_0m
_cod_database_code               7245782
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,
 H5WB), O6W(H6WA,H6WB), O30W(H30A,H30B), O7W(H7WA,H7WB), O8W(H8WA,H8WB),
 O9W(H9WA,H9WB), O10W(H10A,H10B), O11W(H11A,H11B), O12W(H12A,H12B), O13W(H13A,
 H13B), O14W(H14A,H14B), O15W(H15A,H15B), O16W(H16A,H16B), O17W(H17A,H17B),
 O18W(H18A,H18B), O19W(H19A,H19B), O28W(H28A,H28B), O20W(H20A,H20B), O29W(H29A,
 H29B), O21W(H21A,H21B), O22W(H22A,H22B), O23W(H23A,H23B), O24W(H24A,H24B),
 O25W(H25A,H25B), O26W(H26A,H26B), O27W(H27A,H27B)
;
_shelx_res_checksum              48392
_shelx_hkl_checksum              98527
_olex2_submission_special_instructions 'No special instructions were received'