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_4323731
_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_analytical     'C48 H36 N4 Ni'
_chemical_formula_structural     'C48 H36 N4 Ni'
_chemical_formula_sum            'C48 H36 N4 Ni'
_chemical_formula_weight         727.52
_chemical_name_common            Ni(II)DEtTPP
_chemical_name_systematic
; 
 (2,3-Diethyl-5,10,15,20-tetraphenylporphyrinato)nickel(II) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.72(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.198(9)
_cell_length_b                   8.385(6)
_cell_length_c                   29.227(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      20
_cell_volume                     3479(3)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'XDISK, SHElXTL Vers. 5.03 (Siemens, 1994)'
_computing_molecular_graphics    'XP, SHElXTL Vers. 5.03 (Siemens, 1994)'
_computing_publication_material  'XCIF, SHElXTL Vers. 5.03 (Siemens, 1994)'
_computing_structure_refinement  'XL, SHElXTL Vers. 5.03 (Siemens, 1994)'
_computing_structure_solution    'XS, SHElXTL Vers. 5.03 (Siemens, 1994)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Siemens 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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4826
_diffrn_reflns_theta_max         54.10
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   'empirical, XABS2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00064(14)
_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_all   1.037
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_obs          0.0870
_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^)+(0.1218P)^2^+12.8264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2452
_refine_ls_wR_factor_obs         0.2124
_reflns_number_observed          2841
_reflns_number_total             4218
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970765g_02.cif
_cod_data_source_block           ms265
_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^)+(0.1218P)^2^+12.8264P] 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^)+(0.1218P)^2^+12.8264P] 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        3479.2(35)
_cod_database_code               4323731