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_7108129
_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 H57 B N5 Rh, C32 H12 B F24'
_chemical_formula_sum            'C76 H69 B2 F24 N5 Rh'
_chemical_formula_weight         1632.90
_chemical_melting_point          ?
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-12-20
_audit_creation_method           CRYSTALS_ver_14.10
_cell_angle_alpha                90
_cell_angle_beta                 93.0899(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7501(1)
_cell_length_b                   14.1549(1)
_cell_length_c                   21.1993(2)
_cell_measurement_reflns_used    8940
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3820.41(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61210
_diffrn_reflns_theta_full        26.972
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         5.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1662.000
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.40
_refine_diff_density_min         -0.98
_refine_ls_extinction_coef       400(120)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9614
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8721
_refine_ls_number_restraints     326
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.0029940
_refine_ls_shift/su_mean         0.0000348
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.12P)^2^ + 5.19P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1930
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1930
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                6947
_reflns_number_total             8721
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.50
_oxford_diffrn_Wilson_scale      9.58
_oxford_refine_ls_r_factor_ref   0.0827
_oxford_refine_ls_scale          0.3123(6)
_oxford_reflns_number_all        8721
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 129ct10
_cod_data_source_file            c2cc33361a.txt
_cod_data_source_block           3-XRD
_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      'P 2/n '
_cod_original_formula_sum        'C76 H69 B2 F24 N5 Rh1'
_cod_database_code               7108129