Crystal structures of 2,3,7,8,12,13,17,18-octabromo-5,10,15,20-tetrakis(pentafluorophenyl)porphyrin as the chloroform monosolvate and tetrahydrofuran monosolvate
Kingsbury, Christopher J.; Flanagan, Keith J.; Kielmann, Marc; Twamley, Brendan; Senge, Mathias O.; Acta Crystallographica Section E 76 (2020) 214–220; doi:10.1107/S2056989020000432

data_2243251
_publ_section_title
;
 Crystal structures of
 2,3,7,8,12,13,17,18-octabromo-5,10,15,20-tetrakis(pentafluorophenyl)porphyrin
 as the chloroform monosolvate and tetrahydrofuran monosolvate
;
_journal_coeditor_code           TX2016
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              214
_journal_page_last               220
_journal_paper_doi               10.1107/S2056989020000432
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C44 H2 Br8 F20 N4, C H Cl3'
_chemical_formula_moiety         'C44 H2 Br8 F20 N4, C H Cl3'
_chemical_formula_sum            'C45 H3 Br8 Cl3 F20 N4'
_chemical_formula_weight         1725.14
_chemical_name_systematic
'2,3,7,8,12,13,17,18-Octabromo-5,10,15,20-tetrakis(pentafluorophenyl)porphyrin chloroform monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.5162(7)
_cell_length_b                   6.8288(3)
_cell_length_c                   24.5631(12)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.54
_cell_measurement_theta_min      2.59
_cell_volume                     2517.6(2)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
<i>Shelxle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEXII area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            107677
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.576
_diffrn_reflns_theta_min         1.357
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.646
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_description       Block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.464
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         18291
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0204
_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^)+(0.0025P)^2^+1.0050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                17164
_reflns_number_total             18291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2016sup1.cif
_cod_data_source_block           1_CHCl3
_cod_database_code               2243251
_shelx_estimated_absorpt_t_min   0.233
_shelx_estimated_absorpt_t_max   0.518
_shelx_hkl_checksum              55233
_shelx_res_checksum              71995
_cod_database_fobs_code 2243251