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_7121101
_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 Li N3 O'
_chemical_formula_sum            'C46 H46 Li N3 O'
_chemical_formula_weight         663.80
_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             2017-10-02
_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                66.18(6)
_cell_angle_beta                 76.98(5)
_cell_angle_gamma                73.37(6)
_cell_formula_units_Z            2
_cell_length_a                   12.023(8)
_cell_length_b                   12.802(10)
_cell_length_c                   13.927(7)
_cell_measurement_reflns_used    274
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      59.9020
_cell_measurement_theta_min      3.8690
_cell_volume                     1864(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  38.00 150.00   84
  2  \w    -89.00  48.00   1.00   10.00    --  -38.50   0.00  90.00  137
  3  \w    -89.00  -5.00   1.00   10.00    --  -38.50 125.00-120.00   84
  4  \w    -93.00 -53.00   1.00   10.00    --  -38.50 125.00  60.00   40
  5  \w     51.00  98.00   1.00   40.00    --  104.50 -94.00  30.00   47
  6  \w     37.00  89.00   1.00   40.00    --  104.50 -30.00-150.00   52
  7  \w    100.00 167.00   1.00   40.00    --  104.50  77.00-150.00   67
  8  \w     34.00  87.00   1.00   40.00    --  104.50 -45.00-180.00   53
  9  \w     57.00 102.00   1.00   40.00    --  104.50 -94.00 -90.00   45
 10  \w     44.00  92.00   1.00   40.00    --  104.50 -94.00  90.00   48
 11  \w     91.00 174.00   1.00   40.00    --  104.50 125.00 -30.00   83
 12  \w     31.00 109.00   1.00   40.00    --  104.50 -94.00 -30.00   78
 13  \w     47.00  90.00   1.00   40.00    --  104.50 -45.00  60.00   43
 14  \w     86.00 178.00   1.00   40.00    --  104.50  30.00 120.00   92
 15  \w     31.00  87.00   1.00   40.00    --  104.50 -30.00 -60.00   56
 16  \w     58.00  86.00   1.00   40.00    --  104.50 -38.00 -34.00   28
 17  \w     81.00 131.00   1.00   40.00    --  104.50  45.00-180.00   50
 18  \w     63.00 120.00   1.00   40.00    --  104.50-125.00-150.00   57
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0189992000
_diffrn_orient_matrix_UB_12      -0.1343811000
_diffrn_orient_matrix_UB_13      0.0453883000
_diffrn_orient_matrix_UB_21      -0.1318098000
_diffrn_orient_matrix_UB_22      0.0104047000
_diffrn_orient_matrix_UB_23      0.0388777000
_diffrn_orient_matrix_UB_31      -0.0207790000
_diffrn_orient_matrix_UB_32      0.0026133000
_diffrn_orient_matrix_UB_33      -0.1062140000
_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  0.0884
_diffrn_reflns_av_unetI/netI     0.2702
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.919
_diffrn_reflns_theta_max         30.919
_diffrn_reflns_theta_min         3.496
_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    0.536
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.949
_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    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1929
_refine_ls_R_factor_gt           0.0967
_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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.2415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                398
_reflns_number_total             1150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08385h2.cif
_cod_data_source_block           lirnln
_cod_depositor_comments
'Adding full bibliography for 7121096--7121101.cif.'
_cod_database_code               7121101
_nottingham_internal_coll_name   LIRNLN
_nottingham_internal_coll_number 16137
_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   30/05/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 01/06/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 01/06/16
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 22/09/17
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 22/09/17
_nottingham_internal_self_validation_date 22/09/17
_nottingham_internal_self_validation_user pcxrn3
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C46 H47 Li N3 O'
_chemical_oxdiff_usercomment
'LIRNLN #16137 GVB-1048 IN FOMBLIN FILM ON MICROMOUNT FOR RN/DLK'
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.911
_reflns_odcompleteness_completeness 99.50
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C42) =
Uanis(C41) = Uanis(C40) = Uanis(C39) = Uanis(C38)
Uanis(C13) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(C21) = Uanis(N2) =
Uanis(N1) = Uanis(C12) = Uanis(C5) = Uanis(C4) = Uanis(C6) = Uanis(C11) =
Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C32) = Uanis(C17) =
Uanis(N3)
Uanis(C15) = Uanis(C14) = Uanis(C16)
Uanis(C19) = Uanis(C18) = Uanis(C20)
Uanis(O1) = Uanis(C46) = Uanis(C45) = Uanis(C44) = Uanis(C43)
Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27) =
Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31)
Uanis(C10) = Uanis(C15) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C6) =
Uanis(C14) = Uanis(C5) = Uanis(C8) = Uanis(C7) = Uanis(C9) = Uanis(N3) =
Uanis(C16) = Uanis(C4) = Uanis(C3) = Uanis(C1) = Uanis(C2) = Uanis(N2) =
Uanis(N1) = Uanis(O1) = Uanis(C18) = Uanis(C19) = Uanis(C17) = Uanis(C20) =
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23) =
Uanis(C22) = Uanis(C21) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32) =
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) =
Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) =
Uanis(C45) = Uanis(C46) = Uanis(Li1)
3. Others
 U11(O1)=U11(N1)=U11(N2)=U11(N3)=U11(C1)=U11(C2)=U11(C3)=U11(C4)=U11(C5)=
 U11(C6)=U11(C7)=U11(C8)=U11(C9)=U11(C10)=U11(C11)=U11(C12)=U11(C13)=U11(C14)=
 U11(C15)=U11(C16)=U11(C17)=U11(C18)=U11(C19)=U11(C20)=U11(C21)=U11(C22)=
 U11(C23)=U11(C24)=U11(C25)=U11(C26)=U11(C27)=U11(C28)=U11(C29)=U11(C30)=
 U11(C31)=U11(C32)=U11(C33)=U11(C34)=U11(C35)=U11(C36)=U11(C37)=U11(C38)=
 U11(C39)=U11(C40)=U11(C41)=U11(C42)=U11(C43)=U11(C44)=U11(C45)=U11(C46)=
 U11(Li1)=FVAR(1)
 U22(O1)=U22(N1)=U22(N2)=U22(N3)=U22(C1)=U22(C2)=U22(C3)=U22(C4)=U22(C5)=
 U22(C6)=U22(C7)=U22(C8)=U22(C9)=U22(C10)=U22(C11)=U22(C12)=U22(C13)=U22(C14)=
 U22(C15)=U22(C16)=U22(C17)=U22(C18)=U22(C19)=U22(C20)=U22(C21)=U22(C22)=
 U22(C23)=U22(C24)=U22(C25)=U22(C26)=U22(C27)=U22(C28)=U22(C29)=U22(C30)=
 U22(C31)=U22(C32)=U22(C33)=U22(C34)=U22(C35)=U22(C36)=U22(C37)=U22(C38)=
 U22(C39)=U22(C40)=U22(C41)=U22(C42)=U22(C43)=U22(C44)=U22(C45)=U22(C46)=
 U22(Li1)=FVAR(2)
 U33(O1)=U33(N1)=U33(N2)=U33(N3)=U33(C1)=U33(C2)=U33(C3)=U33(C4)=U33(C5)=
 U33(C6)=U33(C7)=U33(C8)=U33(C9)=U33(C10)=U33(C11)=U33(C12)=U33(C13)=U33(C14)=
 U33(C15)=U33(C16)=U33(C17)=U33(C18)=U33(C19)=U33(C20)=U33(C21)=U33(C22)=
 U33(C23)=U33(C24)=U33(C25)=U33(C26)=U33(C27)=U33(C28)=U33(C29)=U33(C30)=
 U33(C31)=U33(C32)=U33(C33)=U33(C34)=U33(C35)=U33(C36)=U33(C37)=U33(C38)=
 U33(C39)=U33(C40)=U33(C41)=U33(C42)=U33(C43)=U33(C44)=U33(C45)=U33(C46)=
 U33(Li1)=FVAR(3)
 U23(O1)=U23(N1)=U23(N2)=U23(N3)=U23(C1)=U23(C2)=U23(C3)=U23(C4)=U23(C5)=
 U23(C6)=U23(C7)=U23(C8)=U23(C9)=U23(C10)=U23(C11)=U23(C12)=U23(C13)=U23(C14)=
 U23(C15)=U23(C16)=U23(C17)=U23(C18)=U23(C19)=U23(C20)=U23(C21)=U23(C22)=
 U23(C23)=U23(C24)=U23(C25)=U23(C26)=U23(C27)=U23(C28)=U23(C29)=U23(C30)=
 U23(C31)=U23(C32)=U23(C33)=U23(C34)=U23(C35)=U23(C36)=U23(C37)=U23(C38)=
 U23(C39)=U23(C40)=U23(C41)=U23(C42)=U23(C43)=U23(C44)=U23(C45)=U23(C46)=
 U23(Li1)=FVAR(4)
 U13(O1)=U13(N1)=U13(N2)=U13(N3)=U13(C1)=U13(C2)=U13(C3)=U13(C4)=U13(C5)=
 U13(C6)=U13(C7)=U13(C8)=U13(C9)=U13(C10)=U13(C11)=U13(C12)=U13(C13)=U13(C14)=
 U13(C15)=U13(C16)=U13(C17)=U13(C18)=U13(C19)=U13(C20)=U13(C21)=U13(C22)=
 U13(C23)=U13(C24)=U13(C25)=U13(C26)=U13(C27)=U13(C28)=U13(C29)=U13(C30)=
 U13(C31)=U13(C32)=U13(C33)=U13(C34)=U13(C35)=U13(C36)=U13(C37)=U13(C38)=
 U13(C39)=U13(C40)=U13(C41)=U13(C42)=U13(C43)=U13(C44)=U13(C45)=U13(C46)=
 U13(Li1)=FVAR(5)
 U12(O1)=U12(N1)=U12(N2)=U12(N3)=U12(C1)=U12(C2)=U12(C3)=U12(C4)=U12(C5)=
 U12(C6)=U12(C7)=U12(C8)=U12(C9)=U12(C10)=U12(C11)=U12(C12)=U12(C13)=U12(C14)=
 U12(C15)=U12(C16)=U12(C17)=U12(C18)=U12(C19)=U12(C20)=U12(C21)=U12(C22)=
 U12(C23)=U12(C24)=U12(C25)=U12(C26)=U12(C27)=U12(C28)=U12(C29)=U12(C30)=
 U12(C31)=U12(C32)=U12(C33)=U12(C34)=U12(C35)=U12(C36)=U12(C37)=U12(C38)=
 U12(C39)=U12(C40)=U12(C41)=U12(C42)=U12(C43)=U12(C44)=U12(C45)=U12(C46)=
 U12(Li1)=FVAR(6)
4.a Secondary CH2 refined with riding coordinates:
 C43(H43a,H43b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b)
4.b 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), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41)
4.c 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              12750
_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 2.633
_oxdiff_exptl_absorpt_empirical_full_min 0.592