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_7108127
_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_absolute_configuration ad
_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     direct
_audit_creation_date             10-10-21
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 117.1045(4)
_cell_angle_gamma                90
_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_reflns_used    9007
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7714.23(13)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.051
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66010
_diffrn_reflns_theta_full        26.924
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         5.122
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.834
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.66
_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    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.96
_refine_ls_abs_structure_details 'Flack (1983), 8320 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.487(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9206
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         17099
_refine_ls_number_restraints     686
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.0074376
_refine_ls_shift/su_mean         0.0001781
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
40.8 65.8 40.6 18.1 4.72
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0866
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0866
_reflns_limit_h_max              29
_reflns_limit_h_min              -29
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              -25
_reflns_number_gt                15502
_reflns_number_total             17099
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.73
_oxford_diffrn_Wilson_scale      63.08
_oxford_refine_ls_r_factor_ref   0.0423
_oxford_refine_ls_scale          0.13755(3)
_oxford_reflns_number_all        17099
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 102ct09
_cod_data_source_file            c2cc33361a.txt
_cod_data_source_block           2-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      'C 1 c 1 '
_cod_original_formula_sum        'C76 H70 B2 F24 Ir1 N5'
_cod_database_code               7108127