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_7121096
_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         'C42 H39 N3'
_chemical_formula_sum            'C42 H39 N3'
_chemical_formula_weight         585.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-07
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-25 deposited with the CCDC.
2018-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.756(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.8139(16)
_cell_length_b                   8.5704(4)
_cell_length_c                   13.5865(7)
_cell_measurement_reflns_used    6322
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2120
_cell_measurement_theta_min      4.7120
_cell_volume                     3272.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
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;
  1 omega  -53.00   -6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  131.0000  -27.0000 47

  2 omega -117.00   -4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000   60.0000 113

  3 omega  -50.00   34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -120.0000 84

  4 omega   20.00   58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   57.0000    0.0000 38

  5 omega   27.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   24.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -99.0000   90.0000 56

  7 omega   42.00   98.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   36.00  121.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   83.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   45.0000  -60.0000 75

 10 omega   38.00   91.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000    0.0000 53

 11 omega  127.00  176.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   45.0000  -30.0000 49

 12 omega   36.00   84.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  -90.0000 48

 13 omega   82.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   45.0000   30.0000 95

 14 omega  101.00  128.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000 -120.0000 27

 15 omega   84.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -95.0000  -90.0000 25

 16 omega   61.00   88.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  120.0000 27

 17 omega  149.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000 -120.0000 28

 18 omega   95.00  121.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000   60.0000 26

 19 omega   37.00   69.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -95.0000  -90.0000 32

 20 omega   98.00  124.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   30.0000 26

 21 omega  149.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   30.0000 29

 22 omega   32.00  131.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000  -60.0000 99

 23 omega  112.00  166.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  131.0000  -27.0000 54

 24 omega  105.00  130.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000  -30.0000 25
;
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_diffrn_radiation_monochromator  mirror
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_diffrn_reflns_av_R_equivalents  0.0651
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_diffrn_reflns_limit_h_max       35
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_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    0.528
_exptl_absorpt_correction_T_max  0.976
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
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_exptl_crystal_F_000             1248
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.5806P] where P=(Fo^2^+2Fc^2^)/3'
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_cod_data_source_block           ornall
_cod_depositor_comments
'Adding full bibliography for 7121096--7121101.cif.'
_cod_database_code               7121096
_nottingham_internal_coll_name   ORNALL
_nottingham_internal_coll_number 15684
_nottingham_internal_coll_client RN/DLK
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_nottingham_internal_coll_frame_time '20.0000, 80.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   24/02/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 25/02/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 07/09/2017
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 07/09/2017
_nottingham_internal_refinement_user pcxrn3
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_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C42 H39 N3'
_chemical_oxdiff_usercomment
'ORNALL - #15684 SN-884 IN FOMBLIN FILM ON A MICROMOUNT FOR RN/DLK'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C2(H2), C4(H4), C7(H7), C9(H9), C21(H21), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              42048
_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
_olex2_submission_special_instructions 'No special instructions were received'