Crystal structure of (15,20-bis(2,3,4,5,6-pentafluorophenyl)-5,10-{(pyridine-3,5-diyl)bis[(sulfanediylmethylene)[1,1'-biphenyl]-4',2-diyl]}porphyrinato)nickel(II) dichloromethane <i>x</i>-solvate (<i>x</i> > 1/2) showing a rare CN5 coordination
Gutzeit, Florian; Näther, Christian; Herges, Rainer; Acta Crystallographica Section E 75 (2019) 1180–1184; doi:10.1107/S2056989019009836

data_2243017
_publ_section_title
;
 Crystal structure of
 (15,20-bis(2,3,4,5,6-pentafluorophenyl)-5,10-{(pyridine-3,5-diyl)bis[(sulfanediylmethylene)[1,1'-biphenyl]-4',2-diyl]}porphyrinato)nickel(II)
 dichloromethane <i>x</i>-solvate (<i>x</i> > 1/2) showing a rare CN5
 coordination
;
_journal_coeditor_code           LH5902
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1180
_journal_page_last               1184
_journal_paper_doi               10.1107/S2056989019009836
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni (C63 H31 F10 N5 S2)], 0.5CH2 Cl2'
_chemical_formula_moiety         'C63 H31 F10 N5 Ni S2, 0.5CH2 Cl2'
_chemical_formula_sum            'C63.5 H32 Cl F10 N5 Ni S2'
_chemical_formula_weight         1213.22
_chemical_name_common            Scr-S-Hair-Clip-Porphyrin
_chemical_name_systematic
;(15,20-Bis(2,3,4,5,6-pentafluorophenyl)-5,10-{(pyridine-3,5-diyl)bis[(sulfanediylmethylene)[1,1'-biphenyl]-4',2-diyl]}porphyrinato)nickel(II)
dichloromethane hemisolvate
;
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.9500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0919(3)
_cell_length_b                   22.0127(4)
_cell_length_c                   17.9648(3)
_cell_measurement_reflns_used    55528
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.003
_cell_measurement_theta_min      1.465
_cell_volume                     5559.46(18)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2008)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008) and DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55497
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.003
_diffrn_reflns_theta_min         1.465
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.9320
_exptl_absorpt_correction_T_min  0.8546
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-RED and X-SHAPE; Stoe & Cie, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.658
_refine_diff_density_min         -1.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0758P)^2^+3.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                10733
_reflns_number_total             12087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5902sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C63.50 H32 Cl F10 N5 Ni S2'
_cod_database_code               2243017
_shelx_hkl_checksum              25623
_shelx_res_checksum              89715
_shelx_fab_checksum              81727
_shelxl_version_number           2.014
_cod_database_fobs_code 2243017