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_4323730
_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         'C48 H38 N4'
_chemical_formula_structural     'C48 H38 N4'
_chemical_formula_sum            'C48 H38 N4'
_chemical_formula_weight         670.82
_chemical_name_common            DEtTPP
_chemical_name_systematic
; 
 2,3-Diethyl-5,10,15,20-tetraphenylporphyrin 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.65(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.333(12)
_cell_length_b                   20.664(14)
_cell_length_c                   10.180(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     3632(4)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'XDISK, Shelxtl-Plus, Siemens, 1994'
_computing_molecular_graphics    'XP, Shelxtl-Plus, Siemens, 1994'
_computing_publication_material  'XCIF, Shelxtl-Plus, Siemens, 1994'
_computing_structure_refinement  'XL-94 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       '\w scans'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5627
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    N/A
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.52
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3.78(407)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.792
_refine_ls_goodness_of_fit_obs   0.753
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.791
_refine_ls_restrained_S_obs      0.753
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_obs          0.0515
_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^)+(0.1184P)^2^+6.4631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1598
_refine_ls_wR_factor_obs         0.1374
_reflns_number_observed          3664
_reflns_number_total             4412
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970765g_01.cif
_cod_data_source_block           ms234
_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^)+(0.1184P)^2^+6.4631P] 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^)+(0.1184P)^2^+6.4631P] 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        3631.9(40)
_cod_database_code               4323730