Synthesis of Rhenium Vinylidene and Carbyne Complexes from Reactions of [Re(dppm)3]I with Terminal Alkynes and Alkynols
Chan, Ka Wing; Bai, Wei; Lee, Kui Fun; Lee, Ka-Ho; Sung, Herman H. Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Organometallics 35 (2016) 3520–; doi:10.1021/acs.organomet.6b00568

data_4088936
_publ_section_title
;
 Synthesis of Rhenium Vinylidene and Carbyne Complexes from Reactions of
 [Re(dppm)3]I with Terminal Alkynes and Alkynols
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3520
_journal_paper_doi               10.1021/acs.organomet.6b00568
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C65 H56 I O P4 Re'
_chemical_formula_sum            'C65 H56 I O P4 Re'
_chemical_formula_weight         1290.08
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-22
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.061(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.3640(4)
_cell_length_b                   11.36180(10)
_cell_length_c                   20.4318(3)
_cell_measurement_reflns_used    14658
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.5650
_cell_measurement_theta_min      4.5070
_cell_volume                     5345.80(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.9941
_diffrn_measured_fraction_theta_max 0.6829
_diffrn_measurement_details
;
  1 omega   40.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   30.0000 31

  2 omega   32.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 44

  3 omega  -17.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -38.0000   90.0000 88

  4 omega   73.00  123.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   60.0000 50

  5 omega  -17.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -38.0000 -180.0000 88

  6 omega   -3.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -125.0000  120.0000 94

  7 omega  -71.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   38.0000   60.0000 79

  8 omega -141.00  -84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  120.0000 57

  9 omega   88.00  164.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  120.0000 76

 10 omega   43.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000  -54.5109 106

 11 omega   42.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 26

 12 omega   40.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000    0.0000 31

 13 omega   39.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -180.0000 29

 14 omega   38.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  120.0000 33

 15 omega   39.00   70.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  -60.0000 31

 16 omega   40.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -120.0000 31

 17 omega   86.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000   30.0000 62

 18 omega   40.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  -30.0000 31

 19 omega   48.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000   30.0000 26

 20 omega   38.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -150.0000 33

 21 omega   40.00   71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  150.0000 31

 22 omega   51.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 32

 23 omega   37.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000    0.0000   90.0000 140

 24 omega   79.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000  128.4470 70

 25 omega   42.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000  128.4470 26
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0238685000
_diffrn_orient_matrix_UB_12      -0.0463020000
_diffrn_orient_matrix_UB_13      0.0498200000
_diffrn_orient_matrix_UB_21      -0.0731209000
_diffrn_orient_matrix_UB_22      0.0490596000
_diffrn_orient_matrix_UB_23      -0.0307442000
_diffrn_orient_matrix_UB_31      -0.0211375000
_diffrn_orient_matrix_UB_32      -0.1175859000
_diffrn_orient_matrix_UB_33      -0.0324221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31289
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.52
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    10.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                8202
_reflns_number_total             9469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00568_si_003.cif
_cod_data_source_block           11
_cod_original_cell_volume        5345.80(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4088936
_publcif_datablock.id            {7e82ab76-ef34-4745-9acd-49dd2ed50f44}
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n