Rearrangement of bis(alkylidynyl)phosphines to phospha-acyls.
Colebatch, Annie L.; Han, Yong-Shen; Hill, Anthony F.; Sharma, Manab; Shang, Rong; Ward, Jas S.; Chemical communications (Cambridge, England) 53 (2017) 1832–1835; doi:10.1039/c6cc09764b

data_7119240
_publ_section_title
;
 Rearrangement of bis(alkylidynyl)phosphines to phospha-acyls.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1832
_journal_page_last               1835
_journal_paper_doi               10.1039/c6cc09764b
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C42 H49 B2 N12 O4 P W2'
_chemical_formula_sum            'C42 H49 B2 N12 O4 P W2'
_chemical_formula_weight         1206.23
_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
_audit_creation_date             2016-11-28
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Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
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2016-11-28 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_environment      N~2~
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_diffrn_measured_fraction_theta_full 0.9998
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_diffrn_measurement_details
;
  1 omega  -18.00   98.00   1.0000   82.6350
omega____ theta____ kappa____ phi______ frames
    -       13.9272   77.0000 -120.0000 116

  2 omega  -20.00   95.00   1.0000   82.6350
omega____ theta____ kappa____ phi______ frames
    -       13.9272   77.0000    0.0000 115

  3 omega  -15.00   96.00   1.0000   82.6350
omega____ theta____ kappa____ phi______ frames
    -       13.9272   77.0000  120.0000 111
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_33      -0.0216109000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41274
_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.907
_diffrn_source                   'Enhance (Mo) X-ray Source'
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
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_refine_diff_density_max         2.298
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+49.3460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_depositor_comments
'Adding full bibliography for 7119239--7119242.cif.'
_cod_original_cell_volume        4984.6(4)
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N111, N112, C112, C113, C114, C115, C111
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N131, N132, C132, C133, C134, C135, C131
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C121, C122, N121, N122, C124, C123, C125
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N51, N52, C52, C53, C54, C51, C55
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N11, N12, C12, C13, C14, C11, C15
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N31, N32, C32, C33, C34, C31, C35
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C171, C172, C173, C174, C175, C176
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
N31 \\sim C32 \\sim N32 \\sim C34 \\sim C33 \\sim C31 \\sim C35: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
N11 \\sim N12 \\sim C12 \\sim C13 \\sim C14 \\sim C11 \\sim C15: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
N52 \\sim C52 \\sim C53 \\sim N51 \\sim C54 \\sim C51 \\sim C55: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
N131 \\sim N132 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C131: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N111 \\sim N112 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C111: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C153 \\sim C154 \\sim N152 \\sim N151 \\sim C152 \\sim C155 \\sim C151: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C171 \\sim C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C3) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
4. Rigid body (RIGU) restrains
 O3, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N162, N142, N152, B4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C23(H23), C33(H33), C43(H43), C53(H53), C63(H63), C72(H72),
 C73(H73), C74(H74), C75(H75), C76(H76), C113(H113), C123(H123), C133(H133),
 C143(H143), C153(H153), C163(H163), C172(H172), C173(H173), C174(H174),
 C175(H175), C176(H176)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C45(H45A,
 H45B,H45C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C61(H61A,H61B,H61C),
 C65(H65A,H65B,H65C), C111(H11D,H11E,H11F), C115(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C125(H12D,H12E,H12F), C131(H13A,H13B,H13C), C135(H13D,H13E,H13F),
 C141(H14A,H14B,H14C), C145(H14D,H14E,H14F), C151(H15D,H15E,H15F), C155(H15G,
 H15H,H15I), C161(H16A,H16B,H16C), C165(H16D,H16E,H16F)
;
_shelx_fab_checksum              43280
_olex2_submission_special_instructions 'No special instructions were received'