Structural study of a manganese(II) `picket-fence' porphyrin complex
Yu, Qiang; Li, Xiangjun; Liu, Diansheng; Li, Jianfeng; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615009304

data_2019979
_publ_section_title
;
 Structural study of a manganese(II) `picket-fence' porphyrin complex
;
_journal_coeditor_code           SK3589
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615009304
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] [Mn Cl (C64 H64 N8 O4)], C4 H8 O'
_chemical_formula_moiety
'C18 H36 K N2 O6 +, C64 H64 Cl Mn N8 O4 -, C4 H8 O'
_chemical_formula_sum            'C86 H108 Cl K Mn N10 O11'
_chemical_formula_weight         1587.31
_chemical_name_common
;
(Cryptand-222)potassium chlorido[<i>meso</i>-tetra(\a,\a,\a,\a-<i>o</i>-\
pivalamidophenyl)porphyrinato]manganese tetrahydrofuran monosolvate
;
_chemical_name_systematic
;(4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium
chlorido[<i>meso</i>-5,10,15,20-tetrakis(2-<i>tert</i>-butanamidophenyl)porphyrinato(2-)]manganese(II) tetrahydrofuran monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.378(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2598(3)
_cell_length_b                   21.2990(3)
_cell_length_c                   22.7585(3)
_cell_measurement_reflns_used    17336
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.6553
_cell_measurement_theta_min      2.9586
_cell_volume                     8314.6(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (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      200(2)
_diffrn_detector_area_resol_mean 16.2141
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Agilent Xcalibur (Eos, Gemini)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            65981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         2.965
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2011)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.972
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         18558
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+8.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                14238
_reflns_number_total             18558
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3589sup1.cf
_cod_data_source_block           I
_cod_database_code               2019979
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              84226
_shelx_res_checksum              29169
_shelxl_version_number           2014/6
_cod_database_fobs_code 2019979