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_4116883
_publ_section_title
;
 Neutral Ligands for Selective Chloride Anion Complexation:
 (\a,\a,\a,\a)-5,10,15,20-Tetrakis(2-(arylurea)phenyl)porphyrins
;
_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            'C94.11 H107.25 Br0.75 Cl4 N12.76 O9 S5'
_chemical_formula_weight         1923.50
_chemical_name_systematic
;
 (Cl-por)(Bu4NBr)0.75 .5(Me2SO)
;
_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                98.412(14)
_cell_angle_beta                 93.934(7)
_cell_angle_gamma                106.595(8)
_cell_formula_units_Z            2
_cell_length_a                   14.677(3)
_cell_length_b                   15.853(2)
_cell_length_c                   22.542(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4938.6(13)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 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  0.0847
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33522
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7418
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             2015
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         16755
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_obs          0.0936
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1272P)^2^+16.8348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2841
_refine_ls_wR_factor_obs         0.2276
_reflns_number_observed          9645
_reflns_number_total             16987
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982052i_2.cif
_cod_data_source_block           sd:'3+TBAr.5DMSO'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1272P)^2^+16.8348P] 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^)+(0.1272P)^2^+16.8348P] 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        4938.6(14)
_cod_database_code               4116883