Regioselective 2,3-disubstituted porphyrins: synthesis, spectral, structural and electrochemical properties
Arif, Waseem; Kumar, Ravi; New Journal of Chemistry 47 (2023) 10541–10551; doi:10.1039/D3NJ01288C

data_7062460
_publ_section_title
;
 Regioselective 2,3-disubstituted porphyrins: synthesis, spectral,
 structural and electrochemical properties
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10541
_journal_page_last               10551
_journal_paper_doi               10.1039/D3NJ01288C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C60 H36 Cu N4'
_chemical_formula_sum            'C60 H36 Cu N4'
_chemical_formula_weight         876.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-16 deposited with the CCDC.	2023-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                66.9110(10)
_cell_angle_beta                 82.2880(10)
_cell_angle_gamma                67.6690(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6718(5)
_cell_length_b                   13.6174(7)
_cell_length_c                   15.3876(7)
_cell_measurement_reflns_used    15338
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.7130
_cell_measurement_theta_min      1.5310
_cell_volume                     2080.75(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26123
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.058
_exptl_absorpt_coefficient_mu    0.574
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             906
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform and methanol'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         7277
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0565P)^2^+2.5273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6535
_reflns_number_total             7277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01288c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7062460--7062461.cif.'
_cod_database_code               7062460
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C59) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.5
Uanis(C58) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.4
3.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C23(H23), C37(H37), C50(H50), C57(H57), C58(H58), C49(H49)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12386
_shelx_fab_checksum              57441
_olex2_submission_special_instructions 'No special instructions were received'