Crystal structure of (15,20-bis(2,3,4,5,6-pentafluorophenyl)-5,10-{(4-methylpyridine-3,5-diyl)bis[(sulfanediylmethylene)[1,1'-biphenyl]-4',2-diyl]}porphyrinato)nickel(II) dichloromethane <i>x</i>-solvate (<i>x</i> > 1/2)
Gutzeit, Florian; Neumann, Tjorge; Näther, Christian; Herges, Rainer; Acta Crystallographica Section E 75 (2019) 1558–1563; doi:10.1107/S2056989019012453

data_2243112
_publ_section_title
;
 Crystal structure of
 (15,20-bis(2,3,4,5,6-pentafluorophenyl)-5,10-{(4-methylpyridine-3,5-diyl)bis[(sulfanediylmethylene)[1,1'-biphenyl]-4',2-diyl]}porphyrinato)nickel(II)
 dichloromethane <i>x</i>-solvate (<i>x</i> > 1/2)
;
_journal_coeditor_code           HB7846
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1558
_journal_page_last               1563
_journal_paper_doi               10.1107/S2056989019012453
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni (C64 H33 F10 N5 S2)] [+ solvent]'
_chemical_formula_moiety         'C64 H33 F10 N5 Ni S2 [+ solvent]'
_chemical_formula_sum            'C64 H33 F10 N5 Ni S2'
_chemical_formula_weight         1184.78
_chemical_name_systematic
;
(15,20-Bis(2,3,4,5,6-pentafluorophenyl)-5,10-{(4-methylpyridine-3,5-diyl)\
bis[(sulfanediylmethylene)[1,1'-biphenyl]-4',2-diyl]}porphyrinato)nickel(II)
dichloromethane solvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6269(2)
_cell_length_b                   18.0525(3)
_cell_length_c                   24.9524(6)
_cell_measurement_reflns_used    44396
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.003
_cell_measurement_theta_min      1.392
_cell_volume                     5687.83(19)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44401
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.003
_diffrn_reflns_theta_min         1.392
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.8102
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red and X-Shape; Stoe, 2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.386
_refine_ls_abs_structure_details
;
 Flack <i>x</i> determined using 4043 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.004(7)
_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     740
_refine_ls_number_reflns         12417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.9016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                10468
_reflns_number_total             12417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7846sup1.cif
_cod_data_source_block           I
_cod_database_code               2243112
_shelx_hkl_checksum              53291
_shelx_res_checksum              71402
_shelx_fab_checksum              5501
_shelxl_version_number           2.014
_cod_database_fobs_code 2243112