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_4116882
_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            'C91.32 H97.98 Br0.83 Cl4 N12.83 O7 S3'
_chemical_formula_weight         1791.85
_chemical_name_systematic
;
 (Cl-por)(Bu4NBr)0.83.3(DMSO)
;
_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                93.92(2)
_cell_angle_beta                 96.969(12)
_cell_angle_gamma                115.655(8)
_cell_formula_units_Z            2
_cell_length_a                   15.349(2)
_cell_length_b                   17.651(2)
_cell_length_c                   18.949(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4551.4(10)
_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  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37880
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        'no observable decay'
_diffrn_standards_interval_count 40000
_diffrn_standards_interval_time  900
_diffrn_standards_number         700
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1874
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0023(4)
_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   1.016
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_hydrogen_treatment    'idealized with riding models'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         19835
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_obs          0.0768
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+6.7359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2180
_refine_ls_wR_factor_obs         0.1759
_reflns_number_observed          11362
_reflns_number_total             19838
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982052i_1.cif
_cod_data_source_block           sd:3+TBABr.3DMSO
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+6.7359P] 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^)+(0.0937P)^2^+6.7359P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116882