Synthesis and structural, photophysical, electrochemical redox and axial ligation properties of highly electron deficient perchlorometalloporphyrins and selective CN− sensing by Co(ii) complexes
Chaudhri, Nivedita; Butcher, Ray J.; Sankar, Muniappan; New Journal of Chemistry 42 (2018) 8190–; doi:10.1039/C7NJ04418F

data_7057242
_publ_section_title
;
 Synthesis and structural, photophysical, electrochemical redox and axial
 ligation properties of highly electron deficient
 perchlorometalloporphyrins and selective CN&#x2212; sensing by Co(ii)
 complexes
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8190
_journal_paper_doi               10.1039/C7NJ04418F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C46 H28 Cl7.50 N4.50 O3 Zn'
_chemical_formula_sum            'C46 H28 Cl7.5 N4.5 O3 Zn'
_chemical_formula_weight         1022.97
_chemical_name_common
beta-heptachloro-18-nitro-5,10,15,20-tetraphenylporphyrinatozinc(II)
_chemical_name_systematic
2,3,7,8,12,13,17-octachloro-18-nitro-5,10,15,20-tetraphenylporphyrinatozinc(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-11-11 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                110.246(6)
_cell_angle_beta                 97.020(6)
_cell_angle_gamma                103.619(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4998(7)
_cell_length_b                   14.4853(9)
_cell_length_c                   15.9272(11)
_cell_measurement_reflns_used    14489
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.5350
_cell_measurement_theta_min      2.1310
_cell_volume                     2153.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'Shelxt (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2361
_diffrn_reflns_av_unetI/netI     0.1239
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10605
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purple-black'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       prism
_exptl_crystal_F_000             1034
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform and Methanol'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.068
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10605
_refine_ls_number_restraints     616
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.1121
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2957
_refine_ls_wR_factor_ref         0.3503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6461
_reflns_number_total             10605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04418f2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7057241--7057245.cif.'
_cod_original_formula_sum        'C46 H28 Cl7.50 N4.50 O3 Zn'
_cod_database_code               7057242
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              68981