Neutral Ligands for Selective Chloride Anion Complexation: (α,α,α,α)-5,10,15,20-Tetrakis(2-(arylurea)phenyl)porphyrins
Raymond C. Jagessar; Maoyu Shang; W. Robert Scheidt; Dennis H. Burns; Journal of the American Chemical Society 120 (1998) 11684–11692; doi:10.1021/ja982052i

data_4116884
_publ_section_title
;
 Neutral Ligands for Selective Chloride Anion Complexation:
 (\a,\a,\a,\a)-5,10,15,20-Tetrakis(2-(arylurea)phenyl)porphyrins
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11684
_journal_page_last               11692
_journal_paper_doi               10.1021/ja982052i
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C98 H116 Cl5 N13 O9 S5'
_chemical_formula_weight         1957.59
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.407(15)
_cell_angle_beta                 93.773(7)
_cell_angle_gamma                107.029(8)
_cell_formula_units_Z            2
_cell_length_a                   14.6619(6)
_cell_length_b                   15.8465(14)
_cell_length_c                   22.527(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4917.9(9)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pfugrath, 1987)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL_V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Enraf-Nonius FAST'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34133
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0004(2)
_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   1.019
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    'riding models or bond length restaints'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1196
_refine_ls_number_reflns         16778
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_obs          0.0821
_refine_ls_shift/esd_max         0.060
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+14.7076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2298
_refine_ls_wR_factor_obs         0.1903
_reflns_number_observed          10703
_reflns_number_total             16972
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982052i_3.cif
_cod_data_source_block           sd:3+TBACl.5DMSO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+14.7076P] 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^)+(0.0924P)^2^+14.7076P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap & geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_original_cell_volume        4917.9(8)
_cod_database_code               4116884