Synthesis and Structural Characterization of Nonplanar Tetraphenylporphyrins and Their Metal Complexes with Graded Degrees of β-Ethyl Substitution
Mathias O. Senge; Werner W. Kalisch; Inorganic Chemistry 36 (1997) 6103–6116; doi:10.1021/ic970765g

data_4323744
_publ_section_title
;
 Synthesis and Structural Characterization of Nonplanar
 Tetraphenylporphyrins and Their Metal Complexes with Graded Degrees of
 \b-Ethyl Substitution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6103
_journal_page_last               6116
_journal_paper_doi               10.1021/ic970765g
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C56 H52 N4 Ni'
_chemical_formula_structural     'C56 H52 N4 Ni'
_chemical_formula_sum            'C56 H52 N4 Ni'
_chemical_formula_weight         839.73
_chemical_name_common            Ni(II)HEt-TPP
_chemical_name_systematic
; 
 (2,3,7,8,12,13-Hexaethyl-5,10,15,20-tetraphenylporphyrinato)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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                78.37(2)
_cell_angle_beta                 68.89(2)
_cell_angle_gamma                83.84(2)
_cell_formula_units_Z            2
_cell_length_a                   12.735(3)
_cell_length_b                   12.915(3)
_cell_length_c                   14.007(3)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      22
_cell_volume                     2103.5(9)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'XDISK, SHELXL Vers. 5.03 (Sheldrick, 1994)'
_computing_molecular_graphics    'XP, SHELXL Vers. 5.03 (Sheldrick, 1994)'
_computing_publication_material  'XCIF, SHELXL Vers. 5.03 (Sheldrick, 1994)'
_computing_structure_refinement  'XL, SHELXL Vers. 5.03 (Sheldrick, 1994)'
_computing_structure_solution    'XS, SHELXL Vers. 5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Syntex P21'
_diffrn_measurement_method       '2theta -theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5893
_diffrn_reflns_theta_max         57.07
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     n/d
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.101
_refine_ls_restrained_S_obs      1.050
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_obs          0.0680
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+3.9994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2014
_refine_ls_wR_factor_obs         0.1724
_reflns_number_observed          4603
_reflns_number_total             5643
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970765g_15.cif
_cod_data_source_block           ms273
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'N/D' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+3.9994P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+3.9994P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2103.5(8)
_cod_database_code               4323744