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_7043130
_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         'C18 H12 As F9 N3 O9 P S3, C2 H3 N'
_chemical_formula_sum            'C20 H15 As F9 N4 O9 P S3'
_chemical_formula_weight         828.43
_chemical_melting_point          461
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-05-17 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                87.1950(10)
_cell_angle_beta                 62.1340(10)
_cell_angle_gamma                73.9630(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0563(6)
_cell_length_b                   12.0768(6)
_cell_length_c                   12.0815(6)
_cell_measurement_reflns_used    9490
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.25
_cell_volume                     1487.92(13)
_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      173.15
_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 0.990
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7323
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.762
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  0.7144
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       fragment
_exptl_crystal_F_000             824
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN / Et2O'
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0470P)^2^+0.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6551
_reflns_number_total             7323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01526g2.cif
_cod_data_source_block           mo_vic1637_0m
_cod_depositor_comments
;

2018-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C18 H12 As F9 N3 O9 P S3), 2(C2 H3 N)'
_cod_original_formula_sum        'C40 H30 As2 F18 N8 O18 P2 S6'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1656.86
_cod_database_code               7043130
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.599
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -1(10)
 2(10)
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:
 C5(H5), C10(H10), C15(H15), C4(H4), C12(H12), C2(H2), C9(H9), C7(H7), C8(H8),
 C14(H14), C3(H3), C13(H13)
3.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_olex2_submission_original_sample_id RS9096
_olex2_submission_special_instructions 'No special instructions were received'