Electrophilic Substitution Reactions of Metallabenzynes
Wai Yiu Hung; Bin Liu; Wangge Shou; Ting Bin Wen; Chuan Shi; Herman H.-Y. Sung; Ian D. Williams; Zhenyang Lin; Guochen Jia; Journal of the American Chemical Society 133 (2011) 18350–18360; doi:10.1021/ja207315h

data_4107082
_publ_section_title
;
 Electrophilic Substitution Reactions of Metallabenzynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18350
_journal_page_last               18360
_journal_paper_doi               10.1021/ja207315h
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H35 Cl2 N O3 Os P2, 0.75(C H2 Cl2)'
_chemical_formula_sum            'C42.75 H36.5 Cl3.5 N O3 Os P2'
_chemical_formula_weight         988.44
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-07
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled Aug 21 2011 22:24:35, GUI svn.r3824)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.165(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.725(4)
_cell_length_b                   10.8721(18)
_cell_length_c                   26.968(5)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.030
_cell_measurement_theta_min      2.394
_cell_volume                     7834(2)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics
;
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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14803
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.617
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
"SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1024 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.7728.
The \l/2 correction factor is 0.00.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       bar
_exptl_crystal_F_000             3916
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.805
_refine_diff_density_min         -2.718
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.106(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         8029
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                7170
_reflns_number_total             8029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207315h_si_006.cif
_cod_data_source_block           shou10
_cod_original_formula_sum        'C42.75 H36.50 Cl3.50 N O3 Os P2'
_cod_database_code               4107082