Synthesis of Phosphonium-Substituted Vinylidene Complexes from [HC\τb CCH2PPh3]+: Exploring the Competition between Allene and Vinylidene Formation.
Smith, Elizabeth J.; Pridmore, Natalie E.; Whitwood, Adrian C.; Lynam, Jason M.; Organometallics 33 (2014) 7260–; doi:10.1021/om5010429

data_4084916
_publ_section_title
;
 Synthesis of Phosphonium-Substituted Vinylidene Complexes from [HC\\tb
 CCH2PPh3]+: Exploring the Competition between Allene and Vinylidene
 Formation.
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7260
_journal_paper_doi               10.1021/om5010429
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C39 H60 Cl P3 Rh, C4 H8 O, C24 H20 B'
_chemical_formula_sum            'C67 H88 B Cl O P3 Rh'
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_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
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Rigaku CrystalClear-SM Expert 3.1 b27
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????
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_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
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_diffrn_measurement_details
;
scan:
    Number of images: 108
               Slice: -35.0000 - 73.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -180.0000
                 XTD: 44.9929
              2theta: -17.0607
scan:
    Number of images: 91
               Slice: -69.0000 - 22.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 60.0000
                 XTD: 44.9929
              2theta: -17.0607
scan:
    Number of images: 91
               Slice: -69.0000 - 22.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -120.0000
                 XTD: 44.9929
              2theta: -17.0607
scan:
    Number of images: 67
               Slice: -88.0000 - -21.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 60.0000
                 XTD: 44.9929
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scan:
    Number of images: 18
               Slice: -31.0000 - -13.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 54.0000
                 Phi: 30.0000
                 XTD: 44.9929
              2theta: -17.0607
scan:
    Number of images: 104
               Slice: -31.0000 - 73.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -120.0000
                 XTD: 44.9929
              2theta: -17.0607
scan:
    Number of images: 82
               Slice: -69.0000 - 13.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 120.0000
                 XTD: 44.9929
              2theta: -17.0607
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
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_diffrn_orient_matrix_UB_11      -0.083461
_diffrn_orient_matrix_UB_12      0.015109
_diffrn_orient_matrix_UB_13      0.028241
_diffrn_orient_matrix_UB_21      -0.018306
_diffrn_orient_matrix_UB_22      0.079677
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_diffrn_orient_matrix_UB_31      -0.018378
_diffrn_orient_matrix_UB_32      -0.005231
_diffrn_orient_matrix_UB_33      -0.042922
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.060
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40506
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         3.066
_diffrn_reflns_transf_matrix_11  -0.083461
_diffrn_reflns_transf_matrix_12  0.015109
_diffrn_reflns_transf_matrix_13  0.028241
_diffrn_reflns_transf_matrix_21  -0.018306
_diffrn_reflns_transf_matrix_22  0.079677
_diffrn_reflns_transf_matrix_23  -0.018508
_diffrn_reflns_transf_matrix_31  -0.018378
_diffrn_reflns_transf_matrix_32  -0.005231
_diffrn_reflns_transf_matrix_33  -0.042922
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.45
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       'flat Prism'
_exptl_crystal_F_000             1220
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_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.932
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0487
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_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^)+(0.0266P)^2^+2.3662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11373
_reflns_number_total             13740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5010429_si_002.cif
_cod_data_source_block           '[10]BPh4.thf'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4084912--4084917.cif.
;
_cod_database_code               4084916
_shelxl_version_number           2013-4
_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.a Ternary CH refined with riding coordinates:
 C34(H34), C22(H22), C28(H28), C25(H25), C37(H37), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C64(H64A,H64B), C66(H66A,H66B), C65(H65A,H65B)
2.c Aromatic/amide H refined with riding coordinates:
 C56(H56), C49(H49), C57(H57), C41(H41), C61(H61), C59(H59), C9(H9), C42(H42),
 C62(H62), C54(H54), C8(H8), C12(H12), C60(H60), C5(H5), C53(H53), C63(H63),
 C50(H50), C55(H55), C18(H18), C48(H48), C21(H21), C6(H6), C13(H13), C11(H11),
 C47(H47), C17(H17), C43(H43), C14(H14), C20(H20), C3(H3), C15(H15), C51(H51),
 C44(H44), C7(H7), C19(H19), C45(H45)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C39(H39A,H39B,
 H39C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C24(H24A,H24B,H24C), C30(H30A,
 H30B,H30C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C),
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              32878
_shelx_hkl_checksum              90969
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'