Tris(2-pyridyl)phosphine as a versatile ligand for pnictogen acceptors
Suter, Riccardo; Sinclair, Hannah; Burford, Neil; McDonald, Robert; Ferguson, Michael J.; Schrader, Erik; Dalton Trans.  (2017) –; doi:10.1039/C7DT01526G

data_7043131
_publ_section_title
;
 Tris(2-pyridyl)phosphine as a versatile ligand for pnictogen acceptors
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01526G
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety
'0.5(C18 H12 F9 N3 O9 P S3 Sb), 0.5(C17 H12 F6 N3 O6 P S2 Sb), 0.5(C F3 O3 S), 0.5(C2 H3 N)'
_chemical_formula_sum            'C19 H13.5 F9 N3.5 O9 P S3 Sb'
_chemical_formula_weight         854.73
_chemical_melting_point          ?
_chemical_name_common            'Trispyridylphosphine antimony tris triflate'
_chemical_name_systematic        'Trispyridylphosphine antimony tris triflate'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_measurement_theta_min      3.2740
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_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'XS (Sheldrick, 2008)'
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_diffrn_detector_type            'CCD area detector'
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_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   40.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  179.0000  150.0000 26

  2 omega  -46.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -57.0000 -180.0000 86

  3 omega   -7.00   27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   77.0000   60.0000 34

  4 omega   -7.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -99.0000  150.0000 70

  5 omega  -44.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -38.0000  -90.0000 91

  6 omega  -46.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -57.0000   60.0000 69

  7 omega   -8.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   77.0000  -60.0000 46

  8 omega    1.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   57.0000  -30.0000 90

  9 omega    1.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   57.0000   90.0000 90

 10 omega  -25.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -99.0000   60.0000 89

 11 omega  -25.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -99.0000  -90.0000 89

 12 omega   34.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  179.0000 -150.0000 52

 13 omega    1.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   57.0000 -150.0000 90
;
_diffrn_measurement_device       'kappa-stage diffractometer'
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_diffrn_measurement_method       '\w and \f scans'
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_diffrn_orient_matrix_UB_12      0.0076343000
_diffrn_orient_matrix_UB_13      -0.0101440000
_diffrn_orient_matrix_UB_21      -0.0070088000
_diffrn_orient_matrix_UB_22      0.0552641000
_diffrn_orient_matrix_UB_23      -0.0077602000
_diffrn_orient_matrix_UB_31      0.0092129000
_diffrn_orient_matrix_UB_32      0.0166308000
_diffrn_orient_matrix_UB_33      0.0304106000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58737
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.841
_diffrn_source                   'sealed tube'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
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_exptl_crystal_F_000             3352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN Et2O'
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_exptl_crystal_size_mid          0.22
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_refine_ls_abs_structure_details
;
 Flack x determined using 7167 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(3)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15038
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+4.1850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0391
_refine_ls_wR_factor_ref         0.0392
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_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                14894
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_cod_data_source_file            c7dt01526g2.cif
_cod_data_source_block           rs09177
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5661.34(9)
_cod_original_formula_sum        'C19 H13.50 F9 N3.50 O9 P S3 Sb'
_cod_database_code               7043131
_chemical_oxdiff_formula         'C50 N3 P Sb S3 O9 F9'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.501(8)
 0.499(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C14(H14), C22(H22), C7(H7), C15(H15), C25(H25), C33(H33), C9(H9),
 C21(H21), C28(H28), C8(H8), C20(H20), C10(H10), C31(H31), C13(H13), C23(H23),
 C30(H30), C26(H26), C12(H12), C27(H27), C2(H2), C5(H5), C3(H3), C4(H4)
3.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'