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_7121100
_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         'C50 H55 Li N3 O'
_chemical_formula_sum            'C50 H55 Li N3 O'
_chemical_formula_weight         720.91
_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     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                90
_cell_angle_beta                 105.0737(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.65773(16)
_cell_length_b                   21.7068(3)
_cell_length_c                   14.23975(17)
_cell_measurement_reflns_used    17705
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3710
_cell_measurement_theta_min      3.7960
_cell_volume                     4076.34(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Agilent Diffraction Atlas S2 detector'
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9874
_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    5.00    --  -38.50  38.00  30.00   84
  2  \w   -111.00 -16.00   1.00    5.00    --  -38.50 -38.00 -60.00   95
  3  \w      2.00  98.00   1.00    5.00    --   42.83-125.00   0.00   96
  4  \w     20.00 115.00   1.00    5.00    --   42.83  38.00-150.00   95
  5  \w     24.00 150.00   1.00   20.00    --  104.50 -15.00  60.00  126
  6  \w     30.00  91.00   1.00   20.00    --  104.50 -30.00 -30.00   61
  7  \w     81.00 178.00   1.00   20.00    --  104.50  30.00  60.00   97
  8  \w     30.00  91.00   1.00   20.00    --  104.50 -30.00-150.00   61
  9  \w     33.00  98.00   1.00   20.00    --  104.50 -45.00-180.00   65
 10  \w     33.00  98.00   1.00   20.00    --  104.50 -45.00  90.00   65
 11  \w     30.00  91.00   1.00   20.00    --  104.50 -30.00 -90.00   61
 12  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00-150.00   86
 13  \w      2.00  98.00   1.00    5.00    --   42.83-125.00 150.00   96
 14  \w     20.00 115.00   1.00    5.00    --   42.83  38.00 -60.00   95
 15  \w     16.00 113.00   1.00    5.00    --   42.83  57.00  90.00   97
 16  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00   0.00   86
 17  \w     59.00 178.00   1.00   20.00    --  104.50  15.00-180.00  119
 18  \w     77.00 175.00   1.00   20.00    --  104.50  61.00 -60.00   98
 19  \w     80.00 105.00   1.00   20.00    --  104.50  45.00   0.00   25
 20  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00  90.00   86
 21  \w     77.00 175.00   1.00   20.00    --  104.50  61.00-120.00   98
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0275936000
_diffrn_orient_matrix_UB_12      -0.0464671000
_diffrn_orient_matrix_UB_13      -0.0845461000
_diffrn_orient_matrix_UB_21      0.1039158000
_diffrn_orient_matrix_UB_22      -0.0315030000
_diffrn_orient_matrix_UB_23      0.0380034000
_diffrn_orient_matrix_UB_31      -0.0456925000
_diffrn_orient_matrix_UB_32      -0.0434323000
_diffrn_orient_matrix_UB_33      0.0629216000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.839
_diffrn_reflns_theta_min         3.805
_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    0.526
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.175
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768.000
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8151
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+1.8272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6967
_reflns_number_total             8151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08385h2.cif
_cod_data_source_block           lirnlj
_cod_depositor_comments
'Adding full bibliography for 7121096--7121101.cif.'
_cod_original_cell_volume        4076.34(8)
_cod_database_code               7121100
_nottingham_internal_coll_name   LIRNLJ
_nottingham_internal_coll_number 15977
_nottingham_internal_coll_client RNL/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 5.00, 20.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxrn3
_nottingham_internal_coll_date   19/04/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 20/04/2016
_nottingham_internal_process_user pcxrn3
_nottingham_internal_solution_date 17/06/16
_nottingham_internal_solution_user pcxrn3
_nottingham_internal_refinement_date 17/06/16
_nottingham_internal_refinement_user pcxrn3
_nottingham_internal_self_archive_date 21/09/2017
_nottingham_internal_self_validation_date 21/09/2017
_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     2016/6
_chemical_oxdiff_formula         'C50 H55 N3 Li O'
_chemical_oxdiff_usercomment
'LIRNLJ #15977 GVB-992 IN FOMBLIN FILM ON MICROMOUNT FOR RN/DLK'
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.894
_reflns_odcompleteness_completeness 99.97
_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. Restrained distances
 C11-C10 \\sim C11-C10A
 with sigma of 0.02
 C9A-C10A \\sim C9-C10
 with sigma of 0.02
 C9-C8 \\sim C9A-C8
 with sigma of 0.02
 C26A-C10A \\sim C26-C10
 with sigma of 0.02
 N3A-C26A \\sim N3-C26
 with sigma of 0.02
 N3A-C27A \\sim N3-C27
 with sigma of 0.02
 C36-C27 \\sim C36A-C27A
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A
 with sigma of 0.02
 C35-C34 \\sim C35A-C34A
 with sigma of 0.02
 C34-C33 \\sim C34A-C33A
 with sigma of 0.02
 C33A-C32A \\sim C33-C32
 with sigma of 0.02
 C32A-C31A \\sim C32-C31
 with sigma of 0.02
 C31A-C30A \\sim C31-C30
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C29A-C28A \\sim C29-C28
 with sigma of 0.02
 C28A-C27A \\sim C28-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10A \\sim C9A \\sim C26A \\sim N3A \\sim C27A \\sim C28A \\sim C29A \\sim C30A
\\sim C31A \\sim C36A \\sim C35A \\sim C34A \\sim C33A \\sim C32A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C10A, C9A, C26A, N3A, C27A, C28A, C29A, C30A, C31A, C36A, C35A, C34A, C33A,
 C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C10A)=Sof(C9A)=Sof(H9A)=Sof(C26A)=Sof(H26A)=Sof(N3A)=Sof(C27A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(C36A)=
 Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=Sof(C32A)=
 Sof(H32A)=1-FVAR(1)
 Sof(N3)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C21(H21)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C47(H47a,H47b), C48(H48a,
 H48b), C49(H49a,H49b), C50(H50a,H50b)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C26(H26), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C9A(H9A), C26A(H26A), C28A(H28A), C29A(H29A),
 C30A(H30A), C35A(H35A), C34A(H34A), C33A(H33A), C32A(H32A)
6.d 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), C25(H25a,H25b,H25c)
;
_shelx_res_checksum              97134
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.787