Synthesis, Spectral, and Electrochemical Studies of Electronically Tunable β-Substituted Porphyrins with Mixed Substituent Pattern.
Kumar, Ravi; Sankar, Muniappan; Inorganic chemistry  (2014) 141120083817000–; doi:10.1021/ic501259g

data_4341724
_publ_section_title
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 Synthesis, Spectral, and Electrochemical Studies of Electronically
 Tunable \b-Substituted Porphyrins with Mixed Substituent Pattern.
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_journal_name_full               'Inorganic chemistry'
_journal_page_first              141120083817000
_journal_paper_doi               10.1021/ic501259g
_journal_year                    2014
_chemical_formula_moiety         'C61 H40 N6 Ni O2 '
_chemical_formula_sum            'C61 H40 N6 Ni O2'
_chemical_formula_weight         947.70
_chemical_name_common            ;NiTPP(NO2)Br2(Py);
_chemical_name_systematic
; 
 2-Nitro-5,10,12,13,15,20-diphenylporphyrinato Nickel(II) 
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                109.644(5)
_cell_angle_beta                 99.080(5)
_cell_angle_gamma                94.664(5)
_cell_formula_units_Z            2
_cell_length_a                   11.938(5)
_cell_length_b                   12.248(5)
_cell_length_c                   17.642(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.01
_cell_volume                     2373.8(15)
_computing_cell_refinement       'APEX II SYSTEM SOFTWARE PROGRAMS'
_computing_data_collection       'APEX II SYSTEM SOFTWARE PROGRAMS'
_computing_data_reduction        'APEXII (WINGX) '
_computing_molecular_graphics    'ORTEP3 (WINGX) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'APEX II DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA TWOTHETA'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37728
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 4 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       square
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.0240(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         11581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                6207
_reflns_number_total             11581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501259g_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4341724