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_4106619
_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                 99.4395(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8313(3)
_cell_length_b                   16.5100(3)
_cell_length_c                   22.8482(5)
_cell_measurement_reflns_used    8410
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     5518.96(19)
_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      250(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details
;
Partial data collection was obtained (220 s/\% exposure) - failure of the 
cooling device prevented further data collection on this crystal. 
Completeness to 25\% is 95%.
;
_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      -0.0257594
_diffrn_orient_matrix_UB_12      -0.0506814
_diffrn_orient_matrix_UB_13      0.0146447
_diffrn_orient_matrix_UB_21      -0.0628358
_diffrn_orient_matrix_UB_22      0.0172905
_diffrn_orient_matrix_UB_23      -0.0185442
_diffrn_orient_matrix_UB_31      0.0077398
_diffrn_orient_matrix_UB_32      -0.0283034
_diffrn_orient_matrix_UB_33      -0.0375520
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19244
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         5.13
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.685
_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.
Data was collected at 150 K (345.2\% @ 220 s/\%).
The sample was cooled at 50 K/h to 100 K.
Data was collected at 100 K (345.2\% @ 220 s/\%).
The sample was warmed at 50 K/h to 250 K.
;
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         11401
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0537P)^2^+9.5557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                7261
_reflns_number_total             11401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2047599_si_002_12.cif
_cod_data_source_block           3_250K_duplicate
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4106619