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_4085569
_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         'C48 H88 P2 Cl2 Si2 Os, 1.5 CH2 Cl2'
_chemical_formula_sum            'C49.5 H91 Cl5 Os P2 Si2'
_chemical_formula_weight         1171.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.145(2)
_cell_length_b                   18.337(2)
_cell_length_c                   16.970(2)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      1.57
_cell_volume                     6268.7(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36930
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8033
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6335
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                4937
_reflns_number_total             6335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501181u_si_002.cif
_cod_data_source_block           wtb47
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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.

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
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        6268.6(13)
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C49.50 H91 Cl5 Os P2 Si2'
_cod_database_code               4085569