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_4076411
_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 H54 Cl2 P3 Re'
_chemical_formula_sum            'C38 H54 Cl2 P3 Re'
_chemical_formula_weight         860.82
_space_group_IT_number           14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.130(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.0109(4)
_cell_length_b                   19.2536(5)
_cell_length_c                   21.9965(6)
_cell_measurement_reflns_used    29432
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.4761
_cell_measurement_theta_min      2.8727
_cell_volume                     7970.4(3)
_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
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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
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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
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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      173.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
1 omega   81.00  125.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000  -86.0000 55

2 omega   40.00   66.40   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000    0.0000 33

3 omega  -73.00   25.40   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
-        0.0000  -38.0000   60.0000 123

4 omega -125.00  -74.60   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000 -157.0000   17.0000 63

5 omega -112.00  -25.60   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-      -55.0000  125.0000  -90.0000 108

6 omega  -17.00   71.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  -38.0000 -180.0000 110

7 omega -126.00  -73.20   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      -64.0000 -157.0000  -52.0000 66

8 omega   96.00  124.80   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
-       55.0000  125.0000  150.0000 36

9 omega   80.00  148.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -174.0000 85

10 omega   38.00   70.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -30.0000 40

11 omega   39.00   69.40   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -60.0000 38

12 omega   40.00   76.80   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000  -60.0000 46

13 omega   39.00   68.60   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -180.0000 37

14 omega   38.00   70.80   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  150.0000 41

15 omega   38.00   70.80   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000  -86.0000 41

16 omega   44.00   76.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   60.0000 40

17 omega   39.00   67.80   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  -90.0000 36

18 omega   39.00   68.60   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000  120.0000 37

19 omega   38.00   70.80   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000   90.0000 41

20 omega   94.00  178.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000   50.0000 -120.0000 105

21 omega   38.00   70.80   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -150.0000 41

22 omega   64.00  122.40   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000    0.0000    0.0000 73

23 omega   42.00  132.40   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000   38.0000 113

24 omega   39.00   71.00   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -25.0000 -120.0000 40

25 omega   42.00   75.60   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -50.0000   90.0000 42

26 omega   41.00   66.60   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000 -174.0000 32

27 omega   38.00  147.60   0.8000   12.0000
omega____ theta____ kappa____ phi______ frames
-      110.0000  -92.0000   89.0000 137
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0232643
_diffrn_orient_matrix_UB_12      -0.0441991
_diffrn_orient_matrix_UB_13      0.0574677
_diffrn_orient_matrix_UB_21      -0.0039666
_diffrn_orient_matrix_UB_22      -0.0653252
_diffrn_orient_matrix_UB_23      -0.0401842
_diffrn_orient_matrix_UB_31      0.0783131
_diffrn_orient_matrix_UB_32      0.0097699
_diffrn_orient_matrix_UB_33      -0.0086272
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47903
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    8.509
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.71396
_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_primary    blue
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         13727
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                12058
_reflns_number_total             13727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201184m_si_002.cif
_cod_data_source_block           CHEN80CULT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4076411