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_7044348
_publ_section_title
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 Synthesis and Oxidation of Phosphine Cations&#x2020;
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03175K
_journal_year                    2017
_chemical_formula_moiety         'C37 H42 F2 N3 P, 2(C H2 Cl2), Ag Cl2'
_chemical_formula_sum            'C39 H46 Ag Cl6 F2 N3 P'
_chemical_formula_weight         946.33
_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     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-20
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2017-09-26 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.717(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.377(4)
_cell_length_b                   10.6024(18)
_cell_length_c                   18.089(3)
_cell_measurement_reflns_used    9025
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.42
_cell_volume                     4289.7(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36624
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.632
_diffrn_reflns_theta_min         1.821
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9846
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0388P)^2^+10.0974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7811
_reflns_number_total             9846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03175k2.cif
_cod_data_source_block           7
_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_original_cell_volume        4289.6(12)
_cod_database_code               7044348
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-C5 = Cl4-C5
 1.771 with sigma of 0.01
 Cl3-Cl4
 2.916 with sigma of 0.03
 Cl5-C6 = Cl6-C6
 1.771 with sigma of 0.01
 Cl5-Cl6
 2.916 with sigma of 0.03
 C2S-Cl2A \\sim C2T-Cl2B
 with sigma of 0.02
 C2S-Cl22 \\sim C2T-Cl
 with sigma of 0.02
 Cl2A-Cl22 \\sim Cl2B-Cl
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl4 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Cl5 \\sim Cl6 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C6 \\sim Cl5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl2B, C2T, Cl
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2A, C2S, Cl22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2B, C2T, H2TA, H2TB, Cl
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl3, Cl4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5, Cl6, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl6, Cl5, C6, H6A, H6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C2T)=Sof(H2TA)=Sof(H2TB)=Sof(Cl2B)=Sof(Cl)=1-FVAR(1)
 Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(Cl2A)=Sof(Cl22)=FVAR(1)
 Fixed Sof: Cl3(0.7) Cl4(0.7) C5(0.7) H5A(0.7) H5B(0.7) Cl5(0.3) Cl6(0.3)
 C6(0.3) H6A(0.3) H6B(0.3)
6.a Ternary CH refined with riding coordinates:
 C410(H410), C430(H430), C450(H450)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2S(H2SA,H2SB), C2T(H2TA,H2TB), C5(H5A,H5B), C6(H6A,H6B)
6.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C202(H202),
 C203(H203), C204(H204), C205(H205), C302(H302), C303(H303), C304(H304),
 C305(H305), C306(H306), C402(H402), C404(H404)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C411(H41A,H41B,H41C), C412(H41D,H41E,H41F), C431(H43A,H43B,
 H43C), C432(H43D,H43E,H43F), C451(H45A,H45B,H45C), C452(H45D,H45E,H45F)
;
_shelx_res_checksum              99873
_olex2_submission_special_instructions 'No special instructions were received'