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_7043132
_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_formula_moiety         'C17 H12 F7 N3 O6 P S2 Sb, 2(C2 H3 N)'
_chemical_formula_sum            'C21 H18 F7 N5 O6 P S2 Sb'
_chemical_formula_weight         786.24
_chemical_melting_point          ?
_chemical_name_common
'Trispyridylphosphine antimony fluoride bis triflate'
_chemical_name_systematic
'Trispyridylphosphine antimony fluoride bis triflate'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1583(3)
_cell_length_b                   15.6137(3)
_cell_length_c                   13.3459(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.71
_cell_measurement_theta_min      3.14
_cell_volume                     2936.66(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.05
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1225
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            93719
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.031
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.133
_exptl_absorpt_correction_T_max  0.6617
_exptl_absorpt_correction_T_min  0.1563
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN Et2O'
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.3640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5152
_reflns_number_total             5958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01526g2.cif
_cod_data_source_block           cu_vic1720_0m
_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_database_code               7043132
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.664
_shelx_estimated_absorpt_t_min   0.180
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C10(H10), C15(H15), C9(H9), C12(H12), C13(H13), C14(H14),
 C5(H5), C2(H2), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C21(H,HA,HB), C19(HC,HD,HE)
;
_olex2_submission_special_instructions 'No special instructions were received'