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_4088935
_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 H55 I P4 Re, I, C H2 Cl2'
_chemical_formula_sum            'C66 H57 Cl2 I2 P4 Re'
_chemical_formula_weight         1484.90
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-27
_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                 103.7904(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.59913(8)
_cell_length_b                   25.23414(16)
_cell_length_c                   20.75974(11)
_cell_measurement_reflns_used    17770
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      75.1330
_cell_measurement_theta_min      4.3850
_cell_volume                     5901.10(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.9897
_diffrn_measured_fraction_theta_max 0.9477
_diffrn_measurement_details
;
  1 omega   83.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000 -180.0000 93

  2 omega -117.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0703  -37.0000   90.0000 102

  3 omega  -49.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0703   37.0000   30.0000 84

  4 omega   45.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0703 -125.0000   60.0000 53

  5 omega   40.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000   30.0000 100

  6 omega   38.00  174.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703    0.0000  150.0000 136

  7 omega  -49.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0703   37.0000 -120.0000 84

  8 omega -115.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0703  -57.0000  -60.0000 104

  9 omega   11.00   63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0703   57.0000 -120.0000 52
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0145383000
_diffrn_orient_matrix_UB_12      -0.0103862000
_diffrn_orient_matrix_UB_13      -0.0707606000
_diffrn_orient_matrix_UB_21      0.0542168000
_diffrn_orient_matrix_UB_22      0.0556101000
_diffrn_orient_matrix_UB_23      -0.0013429000
_diffrn_orient_matrix_UB_31      0.1247096000
_diffrn_orient_matrix_UB_32      -0.0229446000
_diffrn_orient_matrix_UB_33      0.0288286000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24445
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         4.01
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.409
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.094
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         10518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+25.9487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                9940
_reflns_number_total             10518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00568_si_003.cif
_cod_data_source_block           10a
_cod_original_cell_volume        5901.10(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4088935
_publcif_datablock.id            {8bfae4a2-fcd9-43f4-bdd8-dd5ab7170621}
_reflns_odcompleteness_completeness 98.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13