Crystal structure of 2,3-dimethoxy-<i>meso</i>-tetrakis(pentafluorophenyl)morpholinochlorin methylene chloride 0.44-solvate
Churchill, Serena B. S.; Sharma, Meenakshi; Brückner, Christian; Zeller, Matthias; Acta Crystallographica Section E 76 (2020) 1222–1228; doi:10.1107/S2056989020009093

data_2243474
_publ_section_title
;
 Crystal structure of
 2,3-dimethoxy-<i>meso</i>-tetrakis(pentafluorophenyl)morpholinochlorin
 methylene chloride 0.44-solvate
;
_journal_coeditor_code           IS5543
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1222
_journal_page_last               1228
_journal_paper_doi               10.1107/S2056989020009093
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C46 H16 F20 N4 O3, 0.44C H2 Cl2'
_chemical_formula_moiety         'C46 H16 F20 N4 O3, 0.44(C H2 Cl2)'
_chemical_formula_sum            'C46.44 H16.88 Cl0.88 F20 N4 O3'
_chemical_formula_weight         1090.00
_chemical_name_systematic
;
2,3-Dimethoxy-<i>meso</i>-tetrakis(pentafluorophenyl)morpholinochlorin
methylene chloride 0.44-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 113.1683(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.1774(10)
_cell_length_b                   15.4767(7)
_cell_length_c                   26.0442(13)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2899
_cell_measurement_theta_min      3.0185
_cell_volume                     8588.9(7)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015) and
<i>shelXle</i>  (H\"ubschle <i>et al</i>., 2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS '
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         3.002
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al</i>., 2015)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             4340
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10495
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0789P)^2^+8.8470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1644
_reflns_number_gt                6698
_reflns_number_total             10495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5543sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243474
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              41523
_shelx_res_checksum              74334
_cod_database_fobs_code 2243474