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_4088934
_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         'C52 H47 I P4 Re, C H2 Cl2, I'
_chemical_formula_sum            'C53 H49 Cl2 I2 P4 Re'
_chemical_formula_weight         1320.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.142(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1612(3)
_cell_length_b                   21.6494(4)
_cell_length_c                   18.7830(4)
_cell_measurement_reflns_used    15888
_cell_measurement_temperature    115(20)
_cell_measurement_theta_max      75.3370
_cell_measurement_theta_min      4.2040
_cell_volume                     4941.78(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      115(20)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  101.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  111.0000  -30.0000 77

  2 omega  102.00  159.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000  -90.0000 57

  3 omega   89.00  172.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   45.0000   30.0000 83

  4 omega   80.00  178.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   60.0000  -61.0000 98

  5 omega   47.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000    0.0000 61

  6 omega   36.00   97.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000    0.0000 61

  7 omega   33.00   85.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -90.0000 52

  8 omega   31.00  107.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  -90.0000 76

  9 omega   34.00  115.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  150.0000 81

 10 omega  -32.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9453  -57.0000  150.0000 101

 11 omega  -46.00   34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453   37.0000   60.0000 80

 12 omega  -96.00   -7.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  125.0000   30.0000 89

 13 omega -115.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -57.0000  -90.0000 104
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1110363000
_diffrn_orient_matrix_UB_12      -0.0337838000
_diffrn_orient_matrix_UB_13      0.0095188000
_diffrn_orient_matrix_UB_21      -0.0455281000
_diffrn_orient_matrix_UB_22      -0.0376363000
_diffrn_orient_matrix_UB_23      0.0619653000
_diffrn_orient_matrix_UB_31      -0.0407437000
_diffrn_orient_matrix_UB_32      -0.0500608000
_diffrn_orient_matrix_UB_33      -0.0530052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27000
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.08
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    17.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0170P)^2^+15.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                8291
_reflns_number_total             8788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00568_si_003.cif
_cod_data_source_block           9e
_cod_database_code               4088934
_publcif_datablock.id            {09120e2c-0ef5-420c-8a5b-7236ef1c029b}
_chemical_oxdiff_formula         'Re1 I2 C Me P4 Ph8 Cl2'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_olex2_date_sample_data_collection 2015-03-27
_olex2_submission_special_instructions 'No special instructions were received'