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_4088933
_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
'C58 H50 I P4 Re, 0.15(C H2 Cl2), 0.4(C4 H10 O)'
_chemical_formula_sum            'C59.75 H54.3 Cl0.3 I O0.4 P4 Re'
_chemical_formula_weight         1226.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.87836(19)
_cell_length_b                   23.55001(14)
_cell_length_c                   18.77362(12)
_cell_measurement_reflns_used    20634
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      75.4530
_cell_measurement_theta_min      4.7620
_cell_volume                     11441.31(13)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   33.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  120.0000 57

  2 omega -117.00  -15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -37.0000  -90.0000 102

  3 omega  -96.00   -2.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  125.0000 -120.0000 94

  4 omega   33.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   90.0000 57

  5 omega   33.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -120.0000 57

  6 omega   33.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -180.0000 57

  7 omega   26.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000   60.0000 82

  8 omega   26.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  120.0000 82

  9 omega   80.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000 -120.0000 25

 10 omega -115.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -57.0000   30.0000 104

 11 omega -115.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9453  -57.0000  150.0000 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      -0.0203036000
_diffrn_orient_matrix_UB_12      0.0613188000
_diffrn_orient_matrix_UB_13      0.0058932000
_diffrn_orient_matrix_UB_21      -0.0556314000
_diffrn_orient_matrix_UB_22      -0.0226945000
_diffrn_orient_matrix_UB_23      0.0068623000
_diffrn_orient_matrix_UB_31      0.0060895000
_diffrn_orient_matrix_UB_32      -0.0025498000
_diffrn_orient_matrix_UB_33      0.0815361000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            53269
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_min         4.555
_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    9.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73202
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       needle
_exptl_crystal_F_000             4873
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.091
_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     601
_refine_ls_number_reflns         10109
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+8.7140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8721
_reflns_number_total             10109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00568_si_003.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C59.75 H54.30 Cl0.30 I O0.40 P4 Re'
_cod_database_code               4088933
_chemical_oxdiff_formula         'Re1 I1 P4 ph9 C4 Cl2'
_reflns_odcompleteness_completeness 99.69
_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
2. Restrained distances
 C21S-C22S = C25S-C24S
 1.52 with sigma of 0.02
 C21S-O23S
 2.45 with sigma of 0.04
 Cl2-C1S \\sim Cl1-C1S
 with sigma of 0.02
 P3-C61 \\sim P3-C61A
 with sigma of 0.02
 P2-C31A \\sim P2-C31
 with sigma of 0.02
 O23A-C15S \\sim O23A-C21S
 with sigma of 0.02
 C22S-C21S \\sim C25S-C24S
 with sigma of 0.02
3. Others
 Fixed Sof: C21(0.5) C21A(0.5) C22(0.5) H22(0.5) C22A(0.5) H22A(0.5) C23(0.5)
 H23(0.5) C23A(0.5) H23A(0.5) C24(0.5) H24(0.5) C24A(0.5) H24A(0.5) C25(0.5)
 H25(0.5) C25A(0.5) H25A(0.5) C26(0.5) H26(0.5) C26A(0.5) H26A(0.5) C31A(0.6)
 C31(0.4) C32A(0.6) H32A(0.6) C32(0.4) H32(0.4) C33A(0.6) H33A(0.6) C33(0.4)
 H33(0.4) C34A(0.6) H34A(0.6) C34(0.4) H34(0.4) C35A(0.6) H35A(0.6) C35(0.4)
 H35(0.4) C36A(0.6) H36A(0.6) C36(0.4) H36(0.4) C41A(0.5) C41(0.5) C42A(0.5)
 H42A(0.5) C42(0.5) H42(0.5) C43A(0.5) H43A(0.5) C43(0.5) H43(0.5) C44A(0.5)
 H44A(0.5) C44(0.5) H44(0.5) C45A(0.5) H45A(0.5) C45(0.5) H45(0.5) C46A(0.5)
 H46A(0.5) C46(0.5) H46(0.5) C61(0.5) C61A(0.5) C62(0.5) H62(0.5) C62A(0.5)
 H62A(0.5) C63(0.5) H63(0.5) C63A(0.5) H63A(0.5) C64(0.5) H64(0.5) C64A(0.5)
 H64A(0.5) C65(0.5) H65(0.5) C65A(0.5) H65A(0.5) C66(0.5) H66(0.5) C66A(0.5)
 H66A(0.5) C81(0.45) C81A(0.55) C82(0.45) H82(0.45) C82A(0.55) H82A(0.55)
 C83(0.45) H83(0.45) C83A(0.55) H83A(0.55) C84(0.45) H84(0.45) C84A(0.55)
 H84A(0.55) C85(0.45) H85(0.45) C85A(0.55) H85A(0.55) C86(0.45) H86(0.45)
 C86A(0.55) H86A(0.55) C1S(0.15) Cl1(0.15) Cl2(0.15) C11S(0.25) C12S(0.25)
 O13S(0.25) C14S(0.25) C15S(0.25) C21S(0.15) C22S(0.15) O23S(0.075) O23A(0.075)
 C24S(0.1) C25S(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C22A(H22A), C23(H23), C23A(H23A), C24(H24),
 C24A(H24A), C25(H25), C25A(H25A), C26(H26), C26A(H26A), C32A(H32A), C32(H32),
 C33A(H33A), C33(H33), C34A(H34A), C34(H34), C35A(H35A), C35(H35), C36A(H36A),
 C36(H36), C42A(H42A), C42(H42), C43A(H43A), C43(H43), C44A(H44A), C44(H44),
 C45A(H45A), C45(H45), C46A(H46A), C46(H46), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C62(H62), C62A(H62A), C63(H63), C63A(H63A), C64(H64),
 C64A(H64A), C65(H65), C65A(H65A), C66(H66), C66A(H66A), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C82(H82), C82A(H82A), C83(H83), C83A(H83A),
 C84(H84), C84A(H84A), C85(H85), C85A(H85A), C86(H86), C86A(H86A)
;
_shelx_res_checksum              51070
_shelx_hkl_checksum              30103
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'