Alkyne Metathesis Reactions of Rhenium(V) Carbyne Complexes
Bai, Wei; Lee, Ka-Ho; Sung, Herman H. Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Organometallics 35 (2016) 3808–; doi:10.1021/acs.organomet.6b00653

data_4089028
_publ_section_title
;
 Alkyne Metathesis Reactions of Rhenium(V) Carbyne Complexes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3808
_journal_paper_doi               10.1021/acs.organomet.6b00653
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C28 H38 Cl2 O2 P3 Re'
_chemical_formula_sum            'C28 H38 Cl2 O2 P3 Re'
_chemical_formula_weight         756.59
_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
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.2433(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.69221(14)
_cell_length_b                   32.1562(5)
_cell_length_c                   11.6788(2)
_cell_measurement_reflns_used    8600
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.3500
_cell_measurement_theta_min      5.4830
_cell_volume                     3117.61(9)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   33.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  150.0000 57

  2 omega  -49.00   35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   37.0000  -90.0000 84

  3 omega  -70.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953   57.0000   90.0000 68

  4 omega  -96.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  125.0000  -90.0000 94

  5 omega -115.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6953  -57.0000  120.0000 104

  6 omega   80.00  175.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000  120.0000 95

  7 omega  136.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000   30.0000 42

  8 omega   82.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000   30.0000 33

  9 omega   32.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000  -30.0000 112

 10 omega   82.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000 -180.0000 62

 11 omega   54.00  122.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -125.0000  -30.0000 68

 12 omega   33.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000 -150.0000 57

 13 omega   33.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -30.0000 57

 14 omega   32.00  143.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000  120.0000 111
;
_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      -0.1547778000
_diffrn_orient_matrix_UB_12      0.0263355000
_diffrn_orient_matrix_UB_13      -0.0269239000
_diffrn_orient_matrix_UB_21      -0.0585772000
_diffrn_orient_matrix_UB_22      -0.0187818000
_diffrn_orient_matrix_UB_23      -0.1268781000
_diffrn_orient_matrix_UB_31      -0.0840391000
_diffrn_orient_matrix_UB_32      -0.0353364000
_diffrn_orient_matrix_UB_33      0.0474812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17360
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.493
_diffrn_reflns_theta_min         4.195
_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    10.838
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45753
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0320P)^2^+2.4020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4919
_reflns_number_total             5577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00653_si_003.cif
_cod_data_source_block           complex10
_cod_original_cell_volume        3117.60(9)
_cod_database_code               4089028
_chemical_oxdiff_formula         'Re Cl2 P3 Me6 ph3 C4 O2 '
_reflns_odcompleteness_completeness 99.88
_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:
 C3(H3A,H3B)
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)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              36933
_shelx_hkl_checksum              90446
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-08-06
_olex2_submission_special_instructions 'No special instructions were received'