Dehydrogenation of dimethylamine-borane mediated by Group 1 pincer complexes.
Nolla-Saltiel, Roberto; Geer, Ana M.; Lewis, William; Blake, Alexander J.; Kays, Deborah L.; Chemical communications (Cambridge, England) 54 (2018) 1825–1828; doi:10.1039/c7cc08385h

data_7121098
_publ_section_title
;
 Dehydrogenation of dimethylamine-borane mediated by Group 1 pincer
 complexes.
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1825
_journal_page_last               1828
_journal_paper_doi               10.1039/c7cc08385h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'K, C2 H12 B2 N'
_chemical_formula_sum            'C2 H12 B2 K N'
_chemical_formula_weight         110.85
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.402(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   9.6343(3)
_cell_length_b                   22.8460(8)
_cell_length_c                   13.1641(4)
_cell_measurement_reflns_used    5916
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.2280
_cell_measurement_theta_min      4.9840
_cell_volume                     2896.62(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            'Agilent Diffraction Atlas S2 detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  34.00   1.00   10.00    --  -38.50  38.00  30.00   84
  2  \w    -94.00  -2.00   1.00   10.00    --  -38.50 125.00-180.00   92
  3  \w   -117.00  -2.00   1.00   10.00    --  -38.50 -19.00-150.00  115
  4  \w     33.00  98.00   1.00   40.00    --  104.50 -45.00   0.00   65
  5  \w     30.00  91.00   1.00   40.00    --  104.50 -30.00-180.00   61
  6  \w     30.00  91.00   1.00   40.00    --  104.50 -30.00 -60.00   61
  7  \w     23.00 109.00   1.00   40.00    --  104.50 -94.00-120.00   86
  8  \w     33.00  98.00   1.00   40.00    --  104.50 -45.00-120.00   65
  9  \w     33.00  98.00   1.00   40.00    --  104.50 -45.00  30.00   65
 10  \w     40.00  90.00   1.00   40.00    --  104.50 -30.00-150.00   50
 11  \w     75.00 102.00   1.00   40.00    --  104.50  77.00 -60.00   27
 12  \w    104.00 170.00   1.00   40.00    --  104.50  77.00 -60.00   66
 13  \w     45.00  88.00   1.00   40.00    --  104.50 -94.00-180.00   43
 14  \w     59.00  88.00   1.00   40.00    --  104.50 -30.00  60.00   29
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas S2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1167928000
_diffrn_orient_matrix_UB_12      0.0121518000
_diffrn_orient_matrix_UB_13      0.0750542000
_diffrn_orient_matrix_UB_21      0.0647821000
_diffrn_orient_matrix_UB_22      0.0600678000
_diffrn_orient_matrix_UB_23      0.0252658000
_diffrn_orient_matrix_UB_31      -0.0879614000
_diffrn_orient_matrix_UB_32      0.0281384000
_diffrn_orient_matrix_UB_33      -0.0862326000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16081
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.851
_diffrn_reflns_theta_min         3.870
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.437
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.089
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+4.9101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4208
_reflns_number_total             5696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08385h2.cif
_cod_data_source_block           brnalh
_cod_depositor_comments
'Adding full bibliography for 7121096--7121101.cif.'
_cod_original_cell_volume        2896.63(17)
_cod_database_code               7121098
_nottingham_internal_coll_name   BRNALH
_nottingham_internal_coll_number 17093
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '10.00, 40.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   19/06/2017
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 20/06/2017
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 20/06/2017
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 07/09/2017
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 07/09/2017
_nottingham_internal_self_validation_date 07/09/2017
_nottingham_internal_self_validation_user pcxrn3
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C2 H12 B2 K N'
_chemical_oxdiff_usercomment
'BRNALH #17093 GVB-1367 IN FOMBLIN FILM ON MICROMOUNT FOR RN/DLK'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 N3-C5 \\sim N3A-C5A \\sim N3-C6 \\sim N3A-C6A
 with sigma of 0.02
 N3A-B5A \\sim N3-B5 \\sim N3A-B6A \\sim N3-B6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N3, C5, C6, B5, B6, H5A, H5B, H5C, H6A, H6B, H6C, H5D, H5E, H5F, H6D, H6E,
 H6F, N3A, C6A, B6A, B5A, C5A, H6AA, H6AB, H6AC, H6AD, H6AE, H6AF, H5AA, H5AB,
 H5AC, H5AD, H5AE, H5AF
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N3A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(B6A)=Sof(H6AD)=Sof(H6AE)=
 Sof(H6AF)=Sof(B5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C5A)=Sof(H5AD)=Sof(H5AE)=
 Sof(H5AF)=1-FVAR(1)
 Sof(N3)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(B5)=Sof(H5D)=Sof(H5E)=Sof(H5F)=Sof(B6)=Sof(H6D)=Sof(H6E)=Sof(H6F)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), B1(H1D,H1E,H1F),
 B2(H2D,H2E,H2F), B3(H3D,H3E,H3F), B4(H4D,H4E,H4F), B5(H5D,H5E,H5F), B6(H6D,H6E,
 H6F), B7(H7D,H7E,H7F), B8(H8D,H8E,H8F), C6A(H6AA,H6AB,H6AC), B6A(H6AD,H6AE,
 H6AF), B5A(H5AA,H5AB,H5AC), C5A(H5AD,H5AE,H5AF)
;
_shelx_res_checksum              85475
_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.575
_oxdiff_exptl_absorpt_empirical_full_min 0.434