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_7121097
_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         'C46 H46 N3 Na O, C6 H14'
_chemical_formula_sum            'C52 H60 N3 Na O'
_chemical_formula_weight         766.02
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-20
_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                90.659(7)
_cell_angle_beta                 106.001(7)
_cell_angle_gamma                103.336(7)
_cell_formula_units_Z            2
_cell_length_a                   12.1323(9)
_cell_length_b                   13.7056(11)
_cell_length_c                   14.2286(11)
_cell_measurement_reflns_used    3926
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.9810
_cell_measurement_theta_min      4.4220
_cell_volume                     2205.8(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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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.936
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details
;
  1 omega  -65.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000 -180.0000 97

  2 omega -109.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000   30.0000 97

  3 omega   17.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   57.0000   30.0000 96

  4 omega   31.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000   60.0000 60

  5 omega   31.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  150.0000 60

  6 omega   32.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000   90.0000 106

  7 omega   82.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   30.0000    0.0000 96

  8 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000 -180.0000 84

  9 omega   61.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   15.0000  -30.0000 117

 10 omega   35.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000  -60.0000 86

 11 omega   21.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   38.0000 -150.0000 95

 12 omega   12.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   77.0000 -120.0000 105

 13 omega  -29.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152  -38.0000  -90.0000 95

 14 omega   61.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322   15.0000  150.0000 25
;
_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_UB_11      0.0630433000
_diffrn_orient_matrix_UB_12      0.1079140000
_diffrn_orient_matrix_UB_13      -0.0133529000
_diffrn_orient_matrix_UB_21      0.1203144000
_diffrn_orient_matrix_UB_22      -0.0216538000
_diffrn_orient_matrix_UB_23      0.0517550000
_diffrn_orient_matrix_UB_31      0.0098739000
_diffrn_orient_matrix_UB_32      -0.0362879000
_diffrn_orient_matrix_UB_33      -0.0995606000
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16325
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.591
_diffrn_reflns_theta_min         3.908
_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    0.605
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
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
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.1705
_exptl_crystal_size_mid          0.1299
_exptl_crystal_size_min          0.0856
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1265P)^2^+1.7844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5411
_reflns_number_total             8049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08385h2.cif
_cod_data_source_block           narnlb
_cod_depositor_comments
'Adding full bibliography for 7121096--7121101.cif.'
_cod_database_code               7121097
_nottingham_internal_coll_name   NARNLB
_nottingham_internal_coll_number 16059
_nottingham_internal_coll_client RN/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '5.0000, 20.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   01/05/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 01/05/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 01/05/2016
_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
_nottingham_internal_validation_date 20/10/2017
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 20/10/2017
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C51 H49 N3 Na O'
_chemical_oxdiff_usercomment
'NARNLB #16059 SN-945 in fomblin film on a micromount for RN/DLK'
_reflns_odcompleteness_completeness 93.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C56-C55 \\sim C50-C49
 with sigma of 0.02
 C55-C54 \\sim C48-C49
 with sigma of 0.02
 C58-C54 \\sim C54-C53 \\sim C48-C47 \\sim C48-C52
 with sigma of 0.02
 C56-C54 \\sim C50-C48
 with sigma of 0.02
 C49-C52 \\sim C49-C47 \\sim C55-C53 \\sim C55-C58
 with sigma of 0.02
 C53-C58 \\sim C52-C47
 with sigma of 0.02
 C50-C51 \\sim C56-C57
 with sigma of 0.02
 C57-C55 \\sim C51-C49
 with sigma of 0.02
 C45-C44 \\sim C45A-C44
 with sigma of 0.02
 C46-C45 \\sim C46A-C45A
 with sigma of 0.02
 O1-C46 \\sim O1-C46A
 with sigma of 0.02
 O1-C43 \\sim O1-C46 \\sim O1-C46A
 with sigma of 0.02
 C44-C43 \\sim C46-C45 \\sim C46A-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C53 \\sim C55 \\sim C54 \\sim C56 \\sim C58 \\sim C57 \\sim C50 \\sim C49 \\sim
C48 \\sim C51 \\sim C52 \\sim C47: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim C46A \\sim C46 \\sim C45 \\sim C45A \\sim C44 \\sim C43: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C50, C49, C48, C51, C52, C47, C54, C55, C56, C53, C58, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C46A, C46, C45, C45A, C44, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=
 Sof(H46D)=1-FVAR(1)
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 FVAR(1)
 Fixed Sof: C55(0.5) H55A(0.5) H55B(0.5) C54(0.5) H54(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) H57C(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C58(0.5) H58A(0.5)
 H58B(0.5) H58C(0.5) C49(0.5) H49A(0.5) H49B(0.5) C52(0.5) H52A(0.5) H52B(0.5)
 H52C(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C51(0.5) H51A(0.5) H51B(0.5)
 H51C(0.5) C56(0.5) H56A(0.5) H56B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C48(0.5)
 H48(0.5)
6.a Ternary CH refined with riding coordinates:
 C54(H54), C48(H48)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C44(H44C,H44D), C45(H45A,H45B), C46(H46A,
 H46B), C55(H55A,H55B), C49(H49A,H49B), C56(H56A,H56B), C50(H50A,H50B),
 C45A(H45C,H45D), C46A(H46C,H46D)
6.c Me refined with riding coordinates:
 C51(H51A,H51B,H51C)
6.d 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)
6.e 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), C57(H57A,H57B,H57C), C53(H53A,
 H53B,H53C), C58(H58A,H58B,H58C), C52(H52A,H52B,H52C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              1311
_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
_olex2_submission_special_instructions 'No special instructions were received'