Intermediates in the Rh-catalysed dehydrocoupling of phosphine-borane
Miguel A. Huertos; Andrew S. Weller; Chem.Commun. 48 (2012) 7185–; doi:10.1039/c2cc32696e

data_7107970
_publ_section_title
;
 Intermediates in the Rh-catalysed dehydrocoupling of phosphine-borane
;
_journal_name_full               Chem.Commun.
_journal_page_first              7185
_journal_paper_doi               10.1039/c2cc32696e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety
'C32 H12 B F24, C24 H60 B P3 Rh, 0.5(C6 H4.02 F2)'
_chemical_formula_sum            'C59 H74 B2 F25 P3 Rh'
_chemical_formula_weight         1475.62
_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                87.9016(4)
_cell_angle_beta                 80.6774(4)
_cell_angle_gamma                82.2782(5)
_cell_formula_units_Z            2
_cell_length_a                   12.85870(10)
_cell_length_b                   13.37690(10)
_cell_length_c                   20.23660(20)
_cell_measurement_reflns_used    13191
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     3403.37(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, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23790
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1506
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.54
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         15457
_refine_ls_number_restraints     1028
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+3.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                13086
_reflns_number_total             15457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32696e.txt
_cod_data_source_block           3a
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:
'__diffrn_measurement_device_type' tag replaced with
'_diffrn_measurement_device_type'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not mesoured' 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 
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_cod_original_cell_volume        3403.373(50)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107970