B-Methylated Amine-Boranes: Substituent Redistribution, Catalytic Dehydrogenation, and Facile Metal-Free Hydrogen Transfer Reactions.
Stubbs, Naomi E.; Schäfer, André; Robertson, Alasdair P. M.; Leitao, Erin M.; Jurca, Titel; Sparkes, Hazel A.; Woodall, Christopher H.; Haddow, Mairi F.; Manners, Ian; Inorganic chemistry 54 (2015) 10878–10889; doi:10.1021/acs.inorgchem.5b01946

data_4346691
_publ_section_title
;
 B-Methylated Amine-Boranes: Substituent Redistribution, Catalytic
 Dehydrogenation, and Facile Metal-Free Hydrogen Transfer Reactions.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10878
_journal_page_last               10889
_journal_paper_doi               10.1021/acs.inorgchem.5b01946
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C7 H20 B N'
_chemical_formula_sum            'C7 H20 B N'
_chemical_formula_weight         129.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.214(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8792(2)
_cell_length_b                   15.2145(5)
_cell_length_c                   7.9608(2)
_cell_measurement_reflns_used    5981
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      37.56
_cell_measurement_theta_min      2.68
_cell_volume                     932.72(5)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker Apex II kappa CCDC area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCDC area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31003
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.257
_diffrn_reflns_theta_min         2.677
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.6812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0569 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.9096.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         7760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5025
_reflns_number_total             7760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01946_si_004.cif
_cod_data_source_block           test
_cod_database_code               4346691
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), N2(H2), C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C2(H2A,
 H2B,H2C)
;
_shelx_res_checksum              85381
_shelx_hkl_checksum              41766
_olex2_submission_special_instructions 'No special instructions were received'