The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C~5~H~7~N~2~)[Fe^III^(H~2~O)~4~(SO~4~)~2~]
Bednarchuk, Tamara J.; Hornfeck, Wolfgang; Kinzhybalo, Vasyl; Zhou, Zhengyang; Dušek, Michal; Pietraszko, Adam; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619013155

data_2108552
_publ_section_title
;
 The structures and phase transitions in 4-aminopyridinium
 tetraaquabis(sulfato)iron(III),
 (C~5~H~7~N~2~)[Fe^III^(H~2~O)~4~(SO~4~)~2~]
;
_journal_coeditor_code           DQ5037SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619013155
_journal_volume                  75
_journal_year                    2019
_chemical_formula_sum            'C5 H15 Fe N2 O12 S2'
_chemical_formula_weight         415.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                65.34(3)
_cell_angle_beta                 77.51(3)
_cell_angle_gamma                68.73(3)
_cell_formula_units_Z            4
_cell_length_a                   10.516(4)
_cell_length_b                   11.873(4)
_cell_length_c                   13.099(4)
_cell_measurement_reflns_used    2322
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      29.2810
_cell_measurement_theta_min      2.4010
_cell_volume                     1381.0(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond 2.1c (Brandenburg, 1997)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7895
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.998
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.983
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7895
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5963
_reflns_number_total             7895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dq5037sup1.cif
_cod_data_source_block           PhaseIV
_cod_database_code               2108552
_cod_database_fobs_code          2108552
_shelx_shelxl_version_number     2014/7
_oxdiff_exptl_absorpt_empirical_full_min 0.960
_oxdiff_exptl_absorpt_empirical_full_max 1.065
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              27158
_shelx_hkl_checksum              30530