Stabilization of anti-aromatic and strained five-membered rings with a transition metal
Congqing Zhu; Shunhua Li; Ming Luo; Xiaoxi Zhou; Yufen Niu; Minglian Lin; Jun Zhu; Zexing Cao; Xin Lu; Tingbin Wen; Zhaoxiong Xie; Paul v. R. Schleyer; Haiping Xia; Nature Chemistry 5 (2013) 698–703; doi:10.1038/nchem.1690

data_1552031
_publ_section_title
;
 Stabilization of anti-aromatic and strained five-membered rings with a
 transition metal
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              698
_journal_page_last               703
_journal_paper_doi               10.1038/nchem.1690
_journal_volume                  5
_journal_year                    2013
_chemical_formula_moiety         'C63 H51 B Cl F4 O2 Os P3 S, C4.5H9Cl4.5'
_chemical_formula_sum            'C67.5 H60 B Cl5.5 F4 O2 Os P3 S'
_chemical_formula_weight         1500.11
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.416(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5010(3)
_cell_length_b                   11.5920(3)
_cell_length_c                   41.9630(10)
_cell_measurement_reflns_used    10561
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3057
_cell_measurement_theta_min      2.7795
_cell_volume                     6555.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            31151
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    2.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) 
(compiled Oct 25 2010,18:11:34) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3010
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11514
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+32.6965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                9424
_reflns_number_total             11514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1690-s4.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C67.50 H60 B Cl5.50 F4 O2 Os P3 S'
_cod_database_code               1552031