A moderate distortion of the `picket-fence' porphyrin (cryptand-222)potassium chlorido[<i>meso</i>-α,α,α,α-tetrakis(<i>o</i>-pivalamidophenyl)porphyrinato]ferrate(II) <i>n</i>-hexane monosolvate
Yu, Qiang; Liu, Diansheng; Li, Xiangjun; Li, Jianfeng; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615015478

data_2020104
_publ_section_title
;
 A moderate distortion of the `picket-fence' porphyrin
 (cryptand-222)potassium
 chlorido[<i>meso</i>-\a,\a,\a,\a-tetrakis(<i>o</i>-pivalamidophenyl)porphyrinato]ferrate(II)
 <i>n</i>-hexane monosolvate
;
_journal_coeditor_code           FN3203
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615015478
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] , [Fe (C64 H64 N8 O4) Cl] , C6 H14'
_chemical_formula_moiety
'C18 H36 K N2 O6 +, C64 H64 Cl Fe N8 O4 -, C6 H14'
_chemical_formula_sum            'C88 H114 Cl Fe K N10 O10'
_chemical_formula_weight         1602.29
_chemical_name_common            '[K(222)][Fe(TpivPP)Cl](C6H14)'
_chemical_name_systematic
;
(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium(I)
[5,10,15,20-tetrakis(2-<i>tert</i>-butanamidophenyl)porphyrinato]iron(II)
n-hexane monosolvate
;
_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   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                80.946(4)
_cell_angle_beta                 79.029(4)
_cell_angle_gamma                87.039(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0174(4)
_cell_length_b                   14.3273(8)
_cell_length_c                   24.1557(13)
_cell_measurement_reflns_used    5751
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.4498
_cell_measurement_theta_min      3.0453
_cell_volume                     4366.6(4)
_computing_cell_refinement       'CrysAlisPro (Agilent, 2011)'
_computing_data_collection       'CrysAlisPro (Agilent, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent, 2011)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.2141
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type
'Agilent Xcalibur Gemini diffractometer with Eos detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.510
_diffrn_reflns_theta_min         3.051
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2011)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         18570
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0515P)^2^+5.1988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                11295
_reflns_number_total             18570
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3203sup1.cif
_cod_data_source_block           I
_cod_database_code               2020104
_cod_database_fobs_code          2020104
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-05-07
;
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.955
_shelx_hkl_checksum              78628
_shelx_res_checksum              9097
_shelxl_version_number           2014/6