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_4346689
_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_absolute_configuration unk
_chemical_formula_moiety         'C H8 B N'
_chemical_formula_sum            'C H8 B N'
_chemical_formula_weight         44.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8000(19)
_cell_length_b                   13.708(3)
_cell_length_c                   5.1576(11)
_cell_measurement_reflns_used    2088
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      66.52
_cell_measurement_theta_min      5.55
_cell_volume                     692.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Pt135 CCD area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'Bruker Mircostar Rotating anode'
_diffrn_measurement_device_type  'Rotating anode'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2241
_diffrn_reflns_point_group_measured_fraction_full 0.848
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.551
_diffrn_reflns_theta_min         5.549
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0870 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.7311.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.861
_exptl_crystal_description       block
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.097
_refine_diff_density_min         -0.112
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details
;
 Flack x determined using 187 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.35(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         537
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.1145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.548
_reflns_Friedel_fraction_full    0.691
_reflns_Friedel_fraction_max     0.701
_reflns_number_gt                534
_reflns_number_total             537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01946_si_002.cif
_cod_data_source_block           testo1
_cod_original_cell_volume        692.9(2)
_cod_database_code               4346689
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1H \\sim B1-H1G
 with sigma of 0.01
3.a Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_shelx_res_checksum              28142
_shelx_hkl_checksum              53706
_olex2_submission_special_instructions 'No special instructions were received'