Influence of chloroform on crystalline products yielded in reactions of 5,10,15,20-tetraphenylporphyrin with HCl and copper(II) salts
Aparici Plaza, Luis; Chojnacki, Jaroslaw; Acta Crystallographica Section C 68 (2012) m24–m28; doi:10.1107/S0108270111054102

data_2018347
_publ_section_title
;
 Influence of chloroform on crystalline products yielded in reactions of
 5,10,15,20-tetraphenylporphyrin with HCl and copper(II) salts
;
_journal_coeditor_code           FN3092
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m24
_journal_page_last               m28
_journal_paper_doi               10.1107/S0108270111054102
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C44 H32 N4 2+, 2Cl -, 8C H Cl3'
_chemical_formula_moiety         'C44 H32 N4 2+, 2(Cl -), 8(C H Cl3)'
_chemical_formula_sum            'C52 H40 Cl26 N4'
_chemical_formula_weight         1642.58
_chemical_name_systematic
;
5,10,15,20-tetraphenylporphyrin-21,23-diium dichloride
chloroform octasolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.706(2)
_cell_angle_beta                 82.025(2)
_cell_angle_gamma                76.356(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6031(3)
_cell_length_b                   12.6132(3)
_cell_length_c                   24.5118(6)
_cell_measurement_reflns_used    11928
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.7426
_cell_measurement_theta_min      2.3025
_cell_volume                     3452.31(15)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material
'WinGX (Farrugia, 1999), publCIF (Westrip, 2010) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur Sapphire2 (large Be window)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Mo Ka radiation'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22549
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2006), a multifaceted crystal
model based on expressions derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.319
_refine_diff_density_min         -2.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         12824
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.122
_refine_ls_R_factor_gt           0.095
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1268P)^2^+26.0222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2605
_reflns_number_gt                9236
_reflns_number_total             12824
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3092.cif
_cod_data_source_block           I
_cod_database_code               2018347
_cod_database_fobs_code          2018347