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_7121099
_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         'C84 H76 K2 N6'
_chemical_formula_sum            'C84 H76 K2 N6'
_chemical_formula_weight         1247.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                80.79(2)
_cell_angle_beta                 85.14(2)
_cell_angle_gamma                78.098(18)
_cell_formula_units_Z            1
_cell_length_a                   11.670(3)
_cell_length_b                   11.773(2)
_cell_length_c                   12.928(4)
_cell_measurement_reflns_used    1241
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1180
_cell_measurement_theta_min      4.8520
_cell_volume                     1713.1(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'SIR2004 (Burla et al., 2007)'
_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 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    -93.00 -55.00   1.00   10.00    --  -38.50 125.00   0.00   38
  2  \w    -49.00 -10.00   1.00   10.00    --  -38.50  38.00 150.00   39
  3  \w   -103.00 -24.00   1.00   10.00    --  -38.50 -38.00   0.00   79
  4  \w   -109.00 -15.00   1.00   10.00    --  -38.50 -57.00 150.00   94
  5  \w    -64.00  32.00   1.00   10.00    --  -38.50  57.00 -60.00   96
  6  \w     39.00  67.00   1.00   10.00    --   42.13-125.00   0.00   28
  7  \w     48.00  97.00   1.00   40.00    --  108.63 -45.00 150.00   49
  8  \w     47.00 109.00   1.00   40.00    --  108.63 -95.00   0.00   62
  9  \w     35.00 110.00   1.00   40.00    --  108.63 -95.00  90.00   75
 10  \w     50.00  84.00   1.00   40.00    --  108.63 -30.00  30.00   34
 11  \w     38.00  97.00   1.00   40.00    --  108.63-140.00 -44.00   59
 12  \w     92.00 178.00   1.00   40.00    --  108.63  30.00 -60.00   86
 13  \w     28.00 110.00   1.00   40.00    --  108.63 -95.00-180.00   82
 14  \w     93.00 122.00   1.00   40.00    --  108.63-125.00 -60.00   29
 15  \w     42.00  91.00   1.00   40.00    --  108.63 -30.00 -30.00   49
 16  \w     63.00  92.00   1.00   40.00    --  108.63 -45.00  60.00   29
 17  \w     41.00  88.00   1.00   40.00    --  108.63 -45.00 -30.00   47
 18  \w     49.00  82.00   1.00   40.00    --  108.63 -30.00-120.00   33
 19  \w     50.00  91.00   1.00   40.00    --  108.63 -30.00 -90.00   41
 20  \w     33.00  91.00   1.00   40.00    --  108.63 -95.00 -60.00   58
 21  \w     64.00 178.00   1.00   40.00    --  108.63  15.00-120.00  114
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_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      0.0272983000
_diffrn_orient_matrix_UB_12      -0.0416700000
_diffrn_orient_matrix_UB_13      0.1161111000
_diffrn_orient_matrix_UB_21      0.1260654000
_diffrn_orient_matrix_UB_22      -0.0563510000
_diffrn_orient_matrix_UB_23      -0.0336179000
_diffrn_orient_matrix_UB_31      0.0403263000
_diffrn_orient_matrix_UB_32      0.1156202000
_diffrn_orient_matrix_UB_33      0.0046813000
_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  0.1123
_diffrn_reflns_av_unetI/netI     0.1518
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10407
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.591
_diffrn_reflns_theta_max         66.591
_diffrn_reflns_theta_min         3.877
_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    1.602
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       prism
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.2312
_refine_ls_R_factor_gt           0.1335
_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^)+(0.1246P)^2^+9.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3116
_refine_ls_wR_factor_ref         0.3859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2745
_reflns_number_total             5952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08385h2.cif
_cod_data_source_block           krnalg
_cod_depositor_comments
'Adding full bibliography for 7121096--7121101.cif.'
_cod_database_code               7121099
_nottingham_internal_coll_name   KRNALG
_nottingham_internal_coll_number 16090
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 10.00, 40.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   12/05/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 13/05/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 13/05/2016
_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         'C42 H38 K N3'
_chemical_oxdiff_usercomment
'KRNALG #16090 SN-958 IN FOMBLIN FILM ON A MICROMOUNT FOR RN/DLK'
_reflns_odcompleteness_completeness 98.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C24(H24), C26(H26), C32(H32), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              12503
_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 2.858
_oxdiff_exptl_absorpt_empirical_full_min 0.411