Tuning the [L2RhH3B·NR3]+ interaction using phosphine bite angle. Demonstration by the catalytic formation of polyaminoboranes
Romaeo Dallanegra Alasdair P. M. Robertson Adrian B. Chaplin Ian Manners Andrew S. Weller; Chem.Commun. 47 (2011) 3763–; doi:10.1039/c0cc05460g

data_7106146
_publ_author_name
'Romaeo Dallanegra Alasdair P. M. Robertson Adrian B. Chaplin Ian Manners Andrew S. Weller'
_publ_section_title
;
 Tuning the [L2RhH3B&#x00B7;NR3]+ interaction using phosphine bite angle.
 Demonstration by the catalytic formation of polyaminoboranes
;
_journal_name_full               Chem.Commun.
_journal_page_first              3763
_journal_paper_doi               10.1039/c0cc05460g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C30 H38 B N P2 Rh, C32 H12 B F24, 1.25(C6 H4 F2)'
_chemical_formula_sum            'C69.5 H55 B2 F26.5 N P2 Rh'
_chemical_formula_weight         1594.11
_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                110.1373(6)
_cell_angle_beta                 95.3780(7)
_cell_angle_gamma                99.4374(7)
_cell_formula_units_Z            2
_cell_length_a                   12.9731(2)
_cell_length_b                   17.4492(2)
_cell_length_c                   18.3033(3)
_cell_measurement_reflns_used    15041
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     3786.61(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    'SHELXS-86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26357
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.50
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1605
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1196
_refine_ls_number_reflns         15201
_refine_ls_number_restraints     1688
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0857P)^2^+4.3646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                12968
_reflns_number_total             15201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05460g.txt
_cod_data_source_block           168abc10
_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 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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        3786.61(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C69.50 H55 B2 F26.50 N P2 Rh'
_cod_database_code               7106146