Tris(1,1,1,3,3,3-hexafluoroisopropyl) phosphate
Saaidi, Pierre-Loïc; Jeanneau, Erwann; Hasserodt, Jens; Acta Crystallographica Section E 63 (2007) o3241–o3242; doi:10.1107/S160053680702853X

data_2214127
_publ_section_title
;
 Tris(1,1,1,3,3,3-hexafluoroisopropyl) phosphate
;
_journal_coeditor_code           CS2040
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3241
_journal_page_last               o3242
_journal_paper_doi               10.1107/S160053680702853X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C9 H3 F18 O4 P1'
_chemical_formula_moiety         'C9 H3 F18 O4 P1'
_chemical_formula_sum            'C9 H3 F18 O4 P'
_chemical_formula_weight         548.06
_chemical_name_systematic
;
Tris(1,1,1,3,3,3-hexafluoroisopropyl) phosphate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 107.044(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9045(4)
_cell_length_b                   9.9101(3)
_cell_length_c                   19.1760(5)
_cell_measurement_reflns_used    4008
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.73
_cell_volume                     3434.75(16)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'DIAMOND (Brandenburg et al., 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7697
_diffrn_reflns_theta_full        27.853
_diffrn_reflns_theta_max         27.853
_diffrn_reflns_theta_min         2.222
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.12
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.3
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       47(11)
_refine_ls_extinction_method     'Larson (1970), equation 22'
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3242
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.000472
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince,
1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
2.02 1.91 1.40
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                3242
_reflns_number_total             4071
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            cs2040.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C9 H3 F18 O4 P1'
_cod_database_code               2214127
_cod_database_fobs_code          2214127