Hydrogen Shift Reactions of Rhenium Hydrido Carbyne Complexes
Chen, Jiangxi; Shi, Chuan; Sung, Herman Ho-Yung; Williams, Ian Duncan; Lin, Zhenyang; Jia, Guochen; Organometallics 31 (2012) 1817–; doi:10.1021/om201184m

data_4076412
_publ_section_title
;
 Hydrogen Shift Reactions of Rhenium Hydrido Carbyne Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1817
_journal_paper_doi               10.1021/om201184m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C38 H55 Cl P3 Re'
_chemical_formula_sum            'C38 H55 Cl P3 Re'
_chemical_formula_weight         826.38
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.76930(10)
_cell_length_b                   10.00020(10)
_cell_length_c                   38.8107(4)
_cell_measurement_reflns_used    9291
_cell_measurement_temperature    143
_cell_measurement_theta_max      71.4451
_cell_measurement_theta_min      4.4177
_cell_volume                     3776.66(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
A short history of SHELX (Sheldrick, 2007)/Bruker
;
_diffrn_ambient_temperature      143.0
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
1 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -90.0000 45

2 omega   -4.00   25.25   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -38.0000 -120.0000 39

3 omega  -42.00   -3.75   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -38.0000 -120.0000 51

4 omega  -72.00  -42.75   0.7500    5.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -38.0000 -120.0000 39

5 omega  -70.00   17.00   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000   42.0000  156.0000 116

6 omega -112.00  -18.25   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  125.0000 -150.0000 125

7 omega   25.00  124.75   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000   77.0000   30.0000 133

8 omega   73.00  109.00   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000   60.0000 48

9 omega  -95.00  -53.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000  179.0000   90.0000 55

10 omega   45.00   83.25   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000 -150.0000 51

11 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  120.0000 45

12 omega   86.00  146.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000   32.0000 80

13 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -30.0000 45

14 omega   40.00  146.50   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000  -46.0000 142

15 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -60.0000 45

16 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -120.0000 45

17 omega   38.00   77.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000   32.0000 52

18 omega   40.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -150.0000 41

19 omega   37.00   68.50   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  150.0000 42

20 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   60.0000 45

21 omega   37.00   70.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   90.0000 45

22 omega   38.00   71.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000    0.0000 44

23 omega   42.00  126.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -174.0000 112

24 omega   88.00  145.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000  118.0000 77

25 omega   96.00  174.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000 -120.0000 104

26 omega   38.00   74.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000  118.0000 48

27 omega   28.00  124.00   0.7500    8.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000   77.0000  -30.0000 128
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.1033079
_diffrn_orient_matrix_UB_12      -0.1147559
_diffrn_orient_matrix_UB_13      -0.0031132
_diffrn_orient_matrix_UB_21      0.1119725
_diffrn_orient_matrix_UB_22      0.0824352
_diffrn_orient_matrix_UB_23      0.0208653
_diffrn_orient_matrix_UB_31      -0.0430767
_diffrn_orient_matrix_UB_32      -0.0614456
_diffrn_orient_matrix_UB_33      0.0338004
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22740
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         4.57
_exptl_absorpt_coefficient_mu    8.318
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.68125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.133
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                5643
_reflns_number_total             6785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201184m_si_002.cif
_cod_data_source_block           CHEN95CULT
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076412