The first crystal and molecular structures of hydrated bis(n-perfluoroalkyl)phosphinic acids [H3O]+[(Rf)2PO2]− (Rf = C6F13, C7F15 or C8F17)
Rajendra P. Singh; Brendan Twamley; Jean'ne M. Shreeve; J. Chem. Soc., Dalton Trans.  (2000) 4089–4092; doi:10.1039/b004482m

data_7009938
_publ_section_title
;
 The first crystal and molecular structures of hydrated
 bis(n-perfluoroalkyl)phosphinic acids [H3O]+[(Rf)2PO2]&#x2212;
 (Rf&#x00A0;=&#x00A0;C6F13, C7F15 or C8F17)
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4089
_journal_page_last               4092
_journal_paper_doi               10.1039/b004482m
_journal_year                    2000
_chemical_formula_sum            'C19 H9 F34 O4 P'
_chemical_formula_weight         978.23
_chemical_melting_point          187.5(5)
_chemical_name_common            '[H3O][(F17C8)2PO2] + acetone'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7873(6)
_cell_length_b                   30.1060(16)
_cell_length_c                   9.7817(5)
_cell_measurement_reflns_used    3926
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.35
_cell_volume                     3176.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART 1000'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20573
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        ' < 0.01%'
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.9843
_exptl_absorpt_correction_T_min  0.9166
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G.M. Sheldrick
using the method described by Blessing, R.H.; Acta Cryst.
A51, 1995, 33.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         4113
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+13.5180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1861
_reflns_number_gt                3053
_reflns_number_total             4113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004482m.txt
_cod_data_source_block           bt106
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '187-188' was changed to '187.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7009938