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_7035969
_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         'C18 H4 F20 Mo O4 P2'
_chemical_formula_sum            'C18 H4 F20 Mo O4 P2'
_chemical_formula_weight         822.09
_chemical_name_systematic
;
 [Mo(CO)4{(CF3CF=CF)2PCH2CH2P(CF=CFCF3)2}]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-24
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
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2015-07-08 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.202(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2220(10)
_cell_length_b                   13.9344(7)
_cell_length_c                   18.7749(17)
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_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      27.9430
_cell_measurement_theta_min      4.2530
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
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  1 omega  -94.00  -68.00   1.0000   34.1100
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000  -90.0000 26

  2 omega   -6.00   83.00   1.0000   34.1100
omega____ theta____ kappa____ phi______ frames
    -       18.8601   19.0000 -180.0000 89

  3 omega  -53.00   41.00   1.0000   34.1100
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000  -30.0000 94
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
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_diffrn_orient_matrix_UB_11      0.0630973000
_diffrn_orient_matrix_UB_12      0.0220905000
_diffrn_orient_matrix_UB_13      0.0094401000
_diffrn_orient_matrix_UB_21      -0.0002283000
_diffrn_orient_matrix_UB_22      0.0106204000
_diffrn_orient_matrix_UB_23      -0.0370186000
_diffrn_orient_matrix_UB_31      -0.0312475000
_diffrn_orient_matrix_UB_32      0.0446288000
_diffrn_orient_matrix_UB_33      0.0040827000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5541
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.561
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       blade
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         2595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.6959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1964
_reflns_number_total             2595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02043c1.cif
_cod_data_source_block           argp215
_cod_depositor_comments
'Adding full bibliography for 7035966--7035973.cif.'
_cod_database_code               7035969
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C19H4F20P2Mo1O5
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
;
_shelx_res_checksum              82259
_olex2_date_sample_data_collection 2015-02-11
_olex2_submission_special_instructions 'No special instructions were received'