Perfluoropropenyl-containing phosphines from HFC replacements.
Brisdon, Alan K.; Ali Ghaba, Hana; Beutel, Bernd; Egjandi, Amina; Addaraidi, Arij; Pritchard, Robin G.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19717–19731; doi:10.1039/c5dt02043c

data_7035972
_publ_section_title
;
 Perfluoropropenyl-containing phosphines from HFC replacements.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19717
_journal_page_last               19731
_journal_paper_doi               10.1039/c5dt02043c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C14 H4 F20 O2 P2'
_chemical_formula_sum            'C14 H4 F20 O2 P2'
_chemical_formula_weight         646.11
_chemical_name_systematic        (CF3CF=CF)2P(O)CH2CH2P(O)(CF=CFCF3)2
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-05-20T00:58:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-07-08 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.70(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.566(6)
_cell_length_b                   5.0981(8)
_cell_length_c                   16.835(4)
_cell_measurement_reflns_used    356
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.55
_cell_measurement_theta_min      3.42
_cell_measurement_wavelength     0.7107
_cell_volume                     2048.4(8)
_computing_cell_refinement
'CrysalisPro  Version 1.171.36.28a (Agilent Technologies, 2013)'
_computing_data_collection
'CrysalisPro  Version 1.171.36.28a (Agilent Technologies, 2013)'
_computing_data_reduction
'CrysalisPro  Version 1.171.36.28a (Agilent Technologies, 2013)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'Platon (Spek 2105)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.34
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type
'Agilent Technologies Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.00585
_diffrn_orient_matrix_UB_12      0.01102
_diffrn_orient_matrix_UB_13      0.039458
_diffrn_orient_matrix_UB_21      -0.013714
_diffrn_orient_matrix_UB_22      0.058407
_diffrn_orient_matrix_UB_23      -0.017889
_diffrn_orient_matrix_UB_31      -0.069551
_diffrn_orient_matrix_UB_32      0.000244
_diffrn_orient_matrix_UB_33      -0.001944
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2594
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6352
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
        (compiled Mar 18 2013,11:47:30)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.2709
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.2112
_reflns_number_gt                625
_reflns_number_total             2018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02043c1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7035966--7035973.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7035972
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.98