Synthesis and characterization of (cryptand-222)potassium (2-methylimidazolato)(<i>meso</i>-tetraphenylporphinato)ferrate(II)–2-methylimidazole–tetrahydrofuran (1/1/2)
Wu, Qi; Yao, Zhen; Li, Jianfeng; Acta Crystallographica Section C 73 (2017) –; doi:10.1107/S2053229617009202

data_2020848
_publ_section_title
;
 Synthesis and characterization of (cryptand-222)potassium
 (2-methylimidazolato)(<i>meso</i>-tetraphenylporphinato)ferrate(II)--2-methylimidazole--tetrahydrofuran
 (1/1/2)
;
_journal_coeditor_code           EG3222
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229617009202
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] [Fe (C4 H5 N2) (C44 H28 N4)], C4 H6 N2, 2C4 H8 O'
_chemical_formula_moiety
'C18 H36 K N2 O6 +, C48 H33 Fe N6 -, C4 H6 N2, 2(C4 H8 O)'
_chemical_formula_sum            'C78 H91 Fe K N10 O8'
_chemical_formula_weight         1391.55
_chemical_name_common
;(Cryptand-222)potassium
(2-methylimidazolato)(<i>meso</i>-tetraphenylporphinato)ferrate(II)--2-methylimidazole--tetrahydrofuran (1/1/2)
;
_chemical_name_systematic
;(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium
(2-methylimidazolato)(<i>meso</i>-tetraphenylporphinato)ferrate(II)--2-methylimidazole--tetrahydrofuran (1/1/2)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 91.214(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0866(16)
_cell_length_b                   21.934(3)
_cell_length_c                   24.898(3)
_cell_measurement_reflns_used    9389
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0408
_cell_measurement_theta_min      2.4198
_cell_volume                     7145.2(16)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2013)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
enCIFer (Allen <i>et al.</i>,  2004)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST System with area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            151771
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.171
_diffrn_reflns_theta_min         2.234
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.375
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         15806
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+4.8842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                13209
_reflns_number_total             15806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eg3222sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        7145.1(16)
_cod_database_code               2020848
_cod_database_fobs_code          2020848
_shelx_estimated_absorpt_t_min   0.754
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              12414
_shelx_res_checksum              63661
_shelxl_version_number           2014/6