Synthesis of Alkenyl Ylide Complexes from Reactions of ReOCl2(OEt)(PPh3)2with Alkynols
Poon, Ka Chun; Shi, Chuan; Sung, Herman H.-Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Organometallics 31 (2012) 7085–; doi:10.1021/om3005788

data_4079222
_publ_section_title
;
 Synthesis of Alkenyl Ylide Complexes from Reactions of
 ReOCl2(OEt)(PPh3)2with Alkynols
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7085
_journal_paper_doi               10.1021/om3005788
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C42 H39 Cl2 O2 P2 Re, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H43 Cl6 O2 P2 Re'
_chemical_formula_weight         1064.62
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-05-16
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                70.427(3)
_cell_angle_beta                 82.255(3)
_cell_angle_gamma                80.040(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0637(3)
_cell_length_b                   14.3757(5)
_cell_length_c                   18.2998(6)
_cell_measurement_reflns_used    10248
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.2832
_cell_measurement_theta_min      3.2911
_cell_volume                     2205.17(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -70.00  -36.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 34

  2 omega  -27.00   30.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 57

  3 omega    8.00   71.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -38.0000 -180.0000 63

  4 omega   70.00  126.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  129.0000 -165.0000 56

  5 omega  -18.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000    0.0000 -120.0000 129

  6 omega -121.00  -94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000 -141.0000  172.0000 27

  7 omega -106.00  -15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000  -30.0000 91

  8 omega  -91.00    0.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   77.0000 -180.0000 91

  9 omega   47.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000    0.0000   60.0000 100

 10 omega   88.00  174.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  -90.0000 86

 11 omega   38.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000 -148.0000 27

 12 omega   37.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 34

 13 omega   37.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 34

 14 omega   40.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   90.0000 43

 15 omega   40.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -60.0000 35

 16 omega   38.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  114.0000 110

 17 omega   40.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -120.0000 26

 18 omega   42.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 29

 19 omega   79.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000 -148.0000 69

 20 omega   41.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -30.0000 42

 21 omega   88.00  135.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 47

 22 omega  139.00  173.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -120.0000 34

 23 omega   75.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -32.0000 73

 24 omega   39.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -32.0000 27
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0501797000
_diffrn_orient_matrix_UB_12      0.0344669000
_diffrn_orient_matrix_UB_13      -0.0831922000
_diffrn_orient_matrix_UB_21      0.1595144000
_diffrn_orient_matrix_UB_22      0.0239202000
_diffrn_orient_matrix_UB_23      -0.0332380000
_diffrn_orient_matrix_UB_31      0.0449861000
_diffrn_orient_matrix_UB_32      -0.1068777000
_diffrn_orient_matrix_UB_33      -0.0035068000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13705
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40
_diffrn_source_power             2.0
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    9.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         4.370
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7792
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                7116
_reflns_number_total             7792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005788_si_001.cif
_cod_data_source_block           cool58cult_complex8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2205.17(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079222
_reflns_odcompleteness_completeness 56.50
_reflns_odcompleteness_iscentric 0
_reflns_odcompleteness_theta     68.13