Isolation of a Lewis base stabilized parent phosphenium (PH2(+)) and related species.
Liu, Liu; Ruiz, David A.; Dahcheh, Fatme; Bertrand, Guy; Chemical communications (Cambridge, England) 51 (2015) 12732–12735; doi:10.1039/c5cc05241f

data_7117588
_publ_section_title
;
 Isolation of a Lewis base stabilized parent phosphenium (PH2(+)) and
 related species.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12732
_journal_page_last               12735
_journal_paper_doi               10.1039/c5cc05241f
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         '2(C34.5 H28 N P0.5), 2(C F3 O3 S), H2 O'
_chemical_formula_sum            'C71 H58 F6 N2 O7 P S2'
_chemical_formula_weight         1260.28
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-02 deposited with the CCDC.
2015-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                83.039(2)
_cell_angle_beta                 84.164(2)
_cell_angle_gamma                77.715(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4808(11)
_cell_length_b                   14.6435(11)
_cell_length_c                   15.4095(10)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.396
_cell_measurement_theta_min      2.229
_cell_volume                     3159.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker SMART 6000 CCD'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            59669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.855
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1299 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.7253.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             1310
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         11126
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.7676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9434
_reflns_number_total             11126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05241f2.cif
_cod_data_source_block           Compound2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               7117588
_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. Restrained distances
 C81-S2
 1.82 with sigma of 0.005
 S2-O4 = S2-O5 = S2-O0AA
 1.44 with sigma of 0.005
 C81-F4 = C81-F5 = C81-F6
 1.32 with sigma of 0.005
 O10-H10C = O10-H10A = O10-H10B
 0.95 with sigma of 0.02
 H10A-H10C
 1.45 with sigma of 0.02
 H10C-H10B
 1.45 with sigma of 0.02
 H10A-H10B
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C81) = Uanis(C81A)
Uanis(S2A) = Uanis(S2)
Uanis(S1A) = Uanis(S1)
Uanis(C20) = Uanis(C1A)
4. Rigid body (RIGU) restrains
 S2, S2A, F4A, F5A, F6, F4, F5, F6A, O0AA, O4, O5, O4A, O5A, C81, C81A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F10, F19, C20, F13, S1A, O20, O6, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{S1, F1, F2, F3, O1, O2, O3, C1A} sigma for 1-2: 0.02, 1-3: 0.04
as
{S1A, F10, F13, F19, O6, O7, O20, C20}
6. Others
 Sof(S2A)=Sof(F4)=Sof(F5)=Sof(F6A)=Sof(O4A)=Sof(O5A)=Sof(C81A)=1-FVAR(1)
 Sof(S2)=Sof(F4A)=Sof(F5A)=Sof(F6)=Sof(O4)=Sof(O5)=Sof(C81)=FVAR(1)
 Sof(S1A)=Sof(F10)=Sof(F13)=Sof(F19)=Sof(O6)=Sof(O7)=Sof(O20)=Sof(C20)=1-FVAR(2)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(C1A)=FVAR(2)
 Fixed Sof: P004(0.5) N02B(0.5) N02F(0.5) C02D(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) P003(0.5) N02C(0.5) N028(0.5) C025(0.5) C1(0.5) H1(0.5) C3(0.5)
 H3(0.5) H10A(0.66666) H10B(0.66666) H10C(0.66666)
7.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00T(H00T), C00F(H00F), C00P(H00P)
7.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C01A(H01A), C01B(H01B), C01C(H01C), C01E(H01E), C01F(H01F),
 C01G(H01G), C01H(H01H), C01L(H01L), C01N(H01N), C01P(H01P), C01Q(H01Q),
 C01T(H01T), C01U(H01U), C01Y(H01Y), C013(H013), C016(H016), C022(H022),
 C023(H023), C024(H024), C026(H026), C029(H029), C4(H4), C5(H5), C00U(H00U),
 C00V(H00V), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C01D(H01D), C01I(H01I),
 C01J(H01J), C01K(H01K), C01M(H01M), C01O(H01O), C01S(H01S), C01V(H01V),
 C01X(H01X), C011(H011), C014(H014), C015(H015), C017(H017), C018(H018),
 C019(H019), C020(H020), C021(H021), C1(H1), C3(H3)
7.c Idealised Me refined as rotating group:
 C027(H02A,H02B,H02C), C02H(H02D,H02E,H02F)
;
_shelx_res_checksum              73740
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'