Synthesis and Oxidation of Phosphine Cations†
Mehta, Meera; Johnstone, Tim; Lam, Jolie; Bidraha, Bid; Hermannsdorfer, Andre; Driess, Matthias; Stephan, Douglas W.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03175K

data_7044349
_publ_section_title
;
 Synthesis and Oxidation of Phosphine Cations&#x2020;
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03175K
_journal_year                    2017
_chemical_formula_sum            'C74 H86 Ag3 Cl5 N6 O0 P2'
_chemical_formula_weight         1622.28
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-26 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2421(7)
_cell_length_b                   25.5536(9)
_cell_length_c                   31.5604(11)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.57
_cell_volume                     16264.8(10)
_computing_cell_refinement       'Bruker, APREX-II'
_computing_data_collection       'Bruker, APREX-II'
_computing_data_reduction        'Bruker, SAINT'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  'Bruker, SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            73113
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         1.479
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6624
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         18666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0399P)^2^+47.3408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14516
_reflns_number_total             18666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03175k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7044349
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.963
_exptl_absorpt_special_details
;
 Additional spherical absorption correction applied with \m*r =  0.2000
 \l/2 correction factor = 0.0015
;
_shelx_res_checksum              29588
_shelx_fab_checksum              25637