Rearrangement of Metallabenzynes to Chlorocyclopentadienyl Complexes
Chen, Jiangxi; Lee, Ka-Ho; Wen, Tingbin; Gao, Feng; Sung, Herman H. Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Organometallics 34 (2015) 890–; doi:10.1021/om501181u

data_4085570
_publ_section_title
;
 Rearrangement of Metallabenzynes to Chlorocyclopentadienyl Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              890
_journal_paper_doi               10.1021/om501181u
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C31 H37 Cl2 O Os P Si2, C H2 Cl2'
_chemical_formula_sum            'C32 H39 Cl4 O Os P Si2'
_chemical_formula_weight         858.78
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-24
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                80.454(3)
_cell_angle_beta                 85.670(2)
_cell_angle_gamma                63.066(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2527(3)
_cell_length_b                   12.6046(4)
_cell_length_c                   12.9976(4)
_cell_measurement_reflns_used    10627
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.3523
_cell_measurement_theta_min      3.4453
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega   44.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 26

  2 omega   32.00   68.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 36

  3 omega  -26.00    0.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 26

  4 omega  -66.00  -31.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 35

  5 omega   36.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   30.0000 40

  6 omega   14.00   40.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -30.0000 26

  7 omega -110.00  -35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000 -180.0000 75

  8 omega  -17.00   57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -38.0000   90.0000 74

  9 omega   93.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -180.0000 31

 10 omega   73.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  120.0000 41

 11 omega   15.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   19.0000  -90.0000 113

 12 omega -123.00  -83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  -30.0000 40

 13 omega  -63.00   -4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   38.0000    0.0000 59

 14 omega -110.00  -77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000 -120.0000 33

 15 omega   55.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   30.0000 27

 16 omega   41.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -30.0000 28

 17 omega   39.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 25

 18 omega   80.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -60.0000 52

 19 omega   41.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 30

 20 omega   40.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 25

 21 omega   48.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -60.0000 26

 22 omega   52.00   78.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 26

 23 omega  114.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   38.0000  -30.0000 61

 24 omega   39.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  -60.0000 26

 25 omega   42.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  120.0000 25

 26 omega   40.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000  -60.0000 77

 27 omega  120.00  169.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000  -60.0000 49

 28 omega   39.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  120.0000 65

 29 omega   45.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 25

 30 omega   84.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   38.0000  -30.0000 26

 31 omega   53.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 28

 32 omega   48.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -180.0000 35

 33 omega   40.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  150.0000 27

 34 omega   41.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 36

 35 omega   40.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   30.0000 25

 36 omega   45.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 25

 37 omega   68.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000   58.0000 37

 38 omega   52.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000 -174.0000 88
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0583116000
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_diffrn_orient_matrix_UB_31      0.1214097000
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_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_limit_h_max       14
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_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.878
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.638
_refine_diff_density_min         -2.545
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00491(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0780P)^2^+1.2855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                6007
_reflns_number_total             6046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501181u_si_002.cif
_cod_data_source_block           chen137cult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3086 2015-02-26 13:12:21Z robertas 

 Adding full bibliography for 4085569--4085570.cif.
;
_cod_original_cell_volume        1764.83(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085570
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13