(Cryptand-222)potassium(+) (hydrogensulfido)[5,10,15,20-tetrakis(2-pivalamidophenyl)porphyrinato]ferrate(II)
Dhifet, Mondher; Belkhiria, Mohamed Salah; Daran, Jean-Claude; Nasri, Habib; Acta Crystallographica Section E 65 (2009) m967–m968; doi:10.1107/S1600536809028104

data_2222557
_publ_section_title
;(Cryptand-222)potassium(+)
 (hydrogensulfido)[5,10,15,20-tetrakis(2-pivalamidophenyl)porphyrinato]ferrate(II)
;
_journal_coeditor_code           BG2280
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m967
_journal_page_last               m968
_journal_paper_doi               10.1107/S1600536809028104
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] [Fe (C64 H64 N8 O4) (H S)]'
_chemical_formula_moiety         'C64 H64 Fe N8 O4 S, C18 H36 K N2 O6'
_chemical_formula_sum            'C82 H101 Fe K N10 O10 S'
_chemical_formula_weight         1513.74
_chemical_name_common
Iron(II)(hydrosulfido)-tetrakis(pivalamidophenyl)porphirinate
_chemical_name_systematic
;
(Cryptand-222)potassium(+) (hydrogensulfido)[5,10,15,20-tetrakis(2-
pivalamidophenyl)porphyrinato]ferrate(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.611(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9327(7)
_cell_length_b                   21.5340(7)
_cell_length_c                   22.7670(9)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.90
_cell_measurement_theta_min      2.60
_cell_volume                     8641.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            144342
_diffrn_reflns_theta_full        23.22
_diffrn_reflns_theta_max         23.22
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            'Dark purple'
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         12322
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+5.9377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                10135
_reflns_number_total             12322
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2280.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2222557
_cod_database_fobs_code          2222557