C-C Activation in the Solid State in an Organometallic σ-Complex
Adrian B. Chaplin; Jennifer C. Green; Andrew S. Weller; Journal of the American Chemical Society 133 (2011) 13162–13168; doi:10.1021/ja2047599

data_4106622
_publ_section_title
;
 C-C Activation in the Solid State in an Organometallic \s-Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13162
_journal_page_last               13168
_journal_paper_doi               10.1021/ja2047599
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C32 H12 B F24, C23 H37 Ir P'
_chemical_formula_sum            'C55 H49 B F24 Ir P'
_chemical_formula_weight         1399.92
_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                 99.7008(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.75930(10)
_cell_length_b                   16.4200(2)
_cell_length_c                   22.5220(3)
_cell_measurement_reflns_used    14472
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      5.097
_cell_volume                     5380.11(10)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
Data collected over four omega scans (total 345.2\%) with an exposure time 
of 220 s/\%. 
;
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0001852
_diffrn_orient_matrix_UB_12      -0.0527051
_diffrn_orient_matrix_UB_13      0.0222673
_diffrn_orient_matrix_UB_21      -0.0489002
_diffrn_orient_matrix_UB_22      0.0213436
_diffrn_orient_matrix_UB_23      0.0216473
_diffrn_orient_matrix_UB_31      -0.0483061
_diffrn_orient_matrix_UB_32      -0.0218082
_diffrn_orient_matrix_UB_33      -0.0326286
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24519
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_thermal_history
;
The sample was placed directly into the cool stream at 250 K.
Data was collected at 250 K (345.2\% @ 220 s/\%).
The sample was cooled at 50 K/h to 200 K.
Data was collected at 200 K (345.2\% @ 220 s/\%).
The sample was cooled at 50 K/h to 150 K.
;
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         12752
_refine_ls_number_restraints     663
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0344P)^2^+7.7472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                10050
_reflns_number_total             12752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2047599_si_002_15.cif
_cod_data_source_block           3_150K_modelled
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4106622