Trifluoromethanesulfonate salt of 5,10,15,20-tetrakis(1-benzylpyridin-1-ium-4-yl)-21H,23H-porphyrin and its CaII complex
Salomón-Flores, María K.; Valdes-García, Josue; Martínez-Otero, Diego; Dorazco-González, Alejandro; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S205698902400447X

data_2023139
_publ_section_title
;
 Trifluoromethanesulfonate salt of
 5,10,15,20-tetrakis(1-benzylpyridin-1-ium-4-yl)-21H,23H-porphyrin and its
 CaII complex
;
_journal_coeditor_code           NY2004
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S205698902400447X
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Ca0.10 (C68 H53.81 N8)] (C F3 O3 S)4, 4H2 O'
_chemical_formula_moiety
'C68 H53.81 Ca0.10 N8 4+, 4(C F3 O3 S -), 4(H2 O)'
_chemical_formula_sum            'C72 H61.81 Ca0.1 F12 N8 O16 S4'
_chemical_formula_weight         1655.20
_chemical_name_systematic
;(5,10,15,20-tetrakis(1-benzylpyridin-1-ium-4-yl)-21<i>H</i>,23<i>H</i>-porphyrin)calcium(II)
tetrakis(trifluoromethanesulfonate) tetrahydrate
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90.417(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4506(4)
_cell_length_b                   15.6166(6)
_cell_length_c                   22.3537(9)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.44
_cell_measurement_theta_min      3.45
_cell_volume                     3648.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX2 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick 2008)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50051
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.216
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             1703
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         6684
_refine_ls_number_restraints     1623
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+1.1304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                5995
_reflns_number_total             6684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ny2004.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C72 H61.81 Ca0.10 F12 N8 O16 S4'
_cod_database_code               2023139
_shelx_estimated_absorpt_t_min   0.417
_shelx_estimated_absorpt_t_max   0.736
_shelx_hkl_checksum              5025
_shelx_res_checksum              86767