Amine- and Dimeric Amino-Borane Complexes of the {Rh(PiPr3)2}+ Fragment and Their Relevance to the Transition-Metal-Mediated Dehydrocoupling of Amine-Boranes
Adrian B. Chaplin; Andrew S. Weller; Inorganic Chemistry 49 (2010) 1111–1121; doi:10.1021/ic9020542

data_4314683
_publ_section_title
;
 Amine- and Dimeric Amino-Borane Complexes of the {Rh(PiPr3)2}+ Fragment
 and Their Relevance to the Transition-Metal-Mediated Dehydrocoupling of
 Amine-Boranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1111
_journal_page_last               1121
_journal_paper_doi               10.1021/ic9020542
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H58 B2 N2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C54 H70 B3 F24 N2 P2 Rh'
_chemical_formula_weight         1400.40
_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                73.7772(2)
_cell_angle_beta                 86.7370(3)
_cell_angle_gamma                73.2126(3)
_cell_formula_units_Z            4
_cell_length_a                   12.76990(10)
_cell_length_b                   19.72410(10)
_cell_length_c                   27.1519(2)
_cell_measurement_reflns_used    27448
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     6284.62(8)
_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
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_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44379
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.24
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_refine_diff_density_max         0.764
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00056(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1818
_refine_ls_number_reflns         25462
_refine_ls_number_restraints     1074
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0414P)^2^+7.3982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                20382
_reflns_number_total             25462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9020542_si_002_2.cif
_cod_data_source_block           034abc08
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

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 1569 2011-02-09 13:29:24Z adriana 

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        6284.63(7)
_cod_database_code               4314683