Reversible C-H activation of a P(t)Bu(i)Bu2 ligand to reveal a masked 12 electron [Rh(PR3)2]+ cation.
Sewell, Laura J.; Chaplin, Adrian B.; Abdalla, Joseph A. B.; Weller, Andrew S.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 7437–7439; doi:10.1039/c0dt00449a

data_7026467
_publ_section_title
;
 Reversible C-H activation of a P(t)Bu(i)Bu2 ligand to reveal a masked 12
 electron [Rh(PR3)2]+ cation.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7437
_journal_page_last               7439
_journal_paper_doi               10.1039/c0dt00449a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C24 H56 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C56 H68 B F24 P2 Rh'
_chemical_formula_weight         1372.76
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.1981(3)
_cell_angle_beta                 94.4213(4)
_cell_angle_gamma                118.4125(4)
_cell_formula_units_Z            2
_cell_length_a                   12.88050(10)
_cell_length_b                   13.05280(10)
_cell_length_c                   22.3154(2)
_cell_measurement_reflns_used    15663
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.131
_cell_measurement_theta_min      5.097
_cell_volume                     3136.25(5)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26387
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         14829
_refine_ls_number_restraints     1704
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0891P)^2^+3.6865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                11746
_reflns_number_total             14829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00449a.txt
_cod_data_source_block           153abc10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3136.24(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7026467