Water-Soluble Phosphines. 17.1 Novel Water-Soluble Secondary and Tertiary Phosphines with Disulfonated 1,1'-Biphenyl Backbones and Dibenzophosphole Moieties
Oliver Herd; Dietmar Hoff; Konstantin W. Kottsieper; Christian Liek; Kirsten Wenz; Othmar Stelzer; William S. Sheldrick; Inorganic Chemistry 41 (2002) 5034–5042; doi:10.1021/ic011239z

data_4318542
_publ_section_title
;
 Water-Soluble Phosphines. 17.1 Novel Water-Soluble Secondary and Tertiary
 Phosphines with Disulfonated 1,1'-Biphenyl Backbones and Dibenzophosphole
 Moieties
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5034
_journal_page_last               5042
_journal_paper_doi               10.1021/ic011239z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C18 H16 K2 O9.5 P S2'
_chemical_formula_weight         557.60
_chemical_name_systematic
;
  1-Oxa-1-phenyl-5,5'-bissulfonato-dibenzo[b,d]phosphole-dipotassium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.799(3)
_cell_length_b                   19.246(4)
_cell_length_c                   17.764(4)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      7.5
_cell_volume                     4543.2(18)
_computing_cell_refinement       'Siemens R3m/V'
_computing_data_collection       'Siemens R3m/V'
_computing_data_reduction        XDISK
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL 93'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4 4-circle-diffractometer'
_diffrn_measurement_method       'Profile fitted'
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8284
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.29647
_exptl_absorpt_correction_T_min  0.22624
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.036
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         7918
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_obs          0.0784
_refine_ls_shift/esd_max         -0.034
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+27.2320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2414
_refine_ls_wR_factor_obs         0.1904
_reflns_number_observed          5472
_reflns_number_total             7930
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011239z.cif
_cod_data_source_block           stel29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+27.2320P] 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^)+(0.0919P)^2^+27.2320P] 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_original_cell_volume        4543.4(16)
_cod_database_code               4318542