Dimethylamine borane dehydrogenation chemistry: syntheses, X-ray and neutron diffraction studies of 18-electron aminoborane and 14-electron aminoboryl complexes
Christina Y. Tang; Nicholas Phillips; Joshua I. Bates; Amber L. Thompson; Matthias J. Gutmann; Simon Aldridge; Chem.Commun. 48 (2012) 8096–; doi:10.1039/c2cc33361a

data_7108128
_publ_section_title
;
 Dimethylamine borane dehydrogenation chemistry: syntheses, X-ray and
 neutron diffraction studies of 18-electron aminoborane and 14-electron
 aminoboryl complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8096
_journal_paper_doi               10.1039/c2cc33361a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C44 H58 B Ir N5, C32 H12 B F24'
_chemical_formula_sum            'C76 H70 B2 F24 Ir N5'
_chemical_formula_weight         1723.22
_chemical_melting_point          ?
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Refinement of known model'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.11(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8105(2)
_cell_length_b                   19.0153(2)
_cell_length_c                   19.9792(2)
_cell_measurement_temperature    150(2)
_cell_volume                     7714(7)
_computing_cell_refinement       SXD2001
_computing_data_collection       SXD2001
_computing_data_reduction        SXD2001
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Refinement of known model'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.043
_diffrn_measured_fraction_theta_max 0.043
_diffrn_measurement_device_type  'SXD at ISIS neutron source'
_diffrn_measurement_method       'time-of-flight Laue diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation neutron source'
_diffrn_radiation_type           Neutron
_diffrn_radiation_wavelength     Laue
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7931
_diffrn_reflns_theta_full        82.53
_diffrn_reflns_theta_max         82.53
_diffrn_reflns_theta_min         8.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.5583
_exptl_absorpt_correction_T_min  0.3183
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Calculated using custom ISIS software program SXD-2001.
;
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          9.00
_exptl_crystal_size_mid          4.00
_exptl_crystal_size_min          4.00
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.233
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(17)
_refine_ls_extinction_coef       0.000472(19)
_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   1.274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1638
_refine_ls_number_reflns         7931
_refine_ls_number_restraints     3975
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0921
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.2330
_reflns_number_gt                7931
_reflns_number_total             7931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33361a.txt
_cod_data_source_block           2-Neutron
_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:

'_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_sg_symbol_H-M      'C c'
_cod_database_code               7108128