Hexa-μ-acetato-chlorido(μ-<i>N</i>,2-dioxodobenzene-1-carboximidato)-μ~3~-oxido-tetrairon(III)–water (1/1) and hexa-μ-acetato-(μ-<i>N</i>,2-dioxodobenzene-1-carboximidato)fluorido-μ~3~-oxido-tripyridinetetrairon(III)–pyridine–water (1/1/0.24)
Ward, Cassandra L.; Allen, Matthew J.; Lutter, Jacob C.; Acta Crystallographica Section E 77 (2021) 1003–1009; doi:10.1107/S2056989021009208

data_2243916
_publ_section_title
;
 Hexa-\m-acetato-chlorido(\m-<i>N</i>,2-dioxodobenzene-1-carboximidato)-\m~3~-oxido-tetrairon(III)--water
 (1/1) and
 hexa-\m-acetato-(\m-<i>N</i>,2-dioxodobenzene-1-carboximidato)fluorido-\m~3~-oxido-tripyridinetetrairon(III)--pyridine--water
 (1/1/0.24)
;
_journal_coeditor_code           ZL5012
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1003
_journal_page_last               1009
_journal_paper_doi               10.1107/S2056989021009208
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Fe4 (C2 H3 O2)6 (C7 H4 O3) F O (C5 H5 N)5], C5 H5 N, 0.24H2 O'
_chemical_formula_moiety
'2(C34 H37 F Fe4 N4 O16), C5 H5 N, 0.472(H2 O)'
_chemical_formula_sum            'C73 H79.94 F2 Fe8 N9 O32.47'
_chemical_formula_weight         2087.76
_chemical_melting_point          257
_chemical_name_systematic
'Hexa-\m-acetato-(\m-<i>N</i>,2-dioxodobenzene-1-carboximidato)fluorido-\m~3~-oxido-tripyridinetetrairon(III)--pyridine--water (1/1/0.24)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.676(2)
_cell_length_b                   44.806(3)
_cell_length_c                   12.6056(8)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.21
_cell_volume                     17891(2)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/3</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            102006
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.440
_diffrn_reflns_theta_min         1.575
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       plate
_exptl_crystal_F_000             8534
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.379
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_coef       0.000039(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2018)
;
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0392P)^2^+78.0080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                7012
_reflns_number_total             8265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5012sup1.cif
_cod_data_source_block           1-F
_cod_depositor_comments
'Adding full bibliography for 2243916--2243917.cif.'
_cod_database_code               2243916
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.830
_shelx_hkl_checksum              58113
_shelx_res_checksum              68328