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_4323742
_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         C57H49N5Zn.0.4H2O
_chemical_formula_structural     'C57 H49.8 N5 O0.4 Zn'
_chemical_formula_sum            'C57 H49.8 N5 O0.4 Zn'
_chemical_formula_weight         876.59
_chemical_name_common            Zn(II)tTEtTPP(pyr)
_chemical_name_systematic
; 
 (Pyridine)(2,3,12,13-Tetraethyl-5,10,15,20-tetraphenyl- 
 porphyrinato)zinc(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
_cell_angle_alpha                85.08(3)
_cell_angle_beta                 68.22(3)
_cell_angle_gamma                72.60(3)
_cell_formula_units_Z            2
_cell_length_a                   12.800(4)
_cell_length_b                   13.985(6)
_cell_length_c                   14.152(5)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      21
_cell_volume                     2243.9(16)
_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  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      126(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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6407
_diffrn_reflns_theta_max         57.04
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       n/d
_refine_ls_extinction_method     n/d
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6068
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_obs          0.0596
_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^)+(0.0842P)^2^+5.5966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1615
_refine_ls_wR_factor_obs         0.1486
_reflns_number_observed          5075
_reflns_number_total             6072
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970765g_13.cif
_cod_data_source_block           ms317
_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 
;
_cod_original_cell_volume        2243.9(14)
_cod_original_formula_sum        'C57 H49.80 N5 O0.40 Zn'
_cod_database_code               4323742