Dehydrocoupling of dimethylamine‒borane promoted by manganese(ii) m-terphenyl complexes
Sharpe, Helen R.; Geer, Ana M.; Blundell, Toby J.; Hastings, Fiona R.; Fay, Michael W.; Rance, Graham A.; Lewis, William; Blake, Alexander J.; Kays, Deborah L.; Catalysis Science & Technology 8 (2018) 229–; doi:10.1039/C7CY02086D

data_1548132
_publ_section_title
;
 Dehydrocoupling of dimethylamine--borane promoted by manganese(ii)
 m-terphenyl complexes
;
_journal_issue                   1
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              229
_journal_paper_doi               10.1039/C7CY02086D
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H42 Mn'
_chemical_formula_sum            'C44 H42 Mn'
_chemical_formula_weight         625.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-10-06 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.52378(8)
_cell_length_b                   10.52378(8)
_cell_length_c                   30.7376(4)
_cell_measurement_reflns_used    26735
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.7070
_cell_measurement_theta_min      2.8752
_cell_volume                     3404.19(6)
_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    'ShelXS (Sheldrick, 2008)'
_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 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  27.00   1.00    5.00    --  -43.31  38.00-150.00   77
  2  \w    -50.00  27.00   1.00    5.00    --  -43.31  38.00-180.00   77
  3  \w    -50.00  27.00   1.00    5.00    --  -43.31  38.00 120.00   77
  4  \w     34.00  98.00   1.00   20.00    --  103.00 -45.00-120.00   64
  5  \w     30.00  91.00   1.00   20.00    --  103.00 -30.00-180.00   61
  6  \w     30.00  91.00   1.00   20.00    --  103.00 -30.00 120.00   61
  7  \w     30.00  91.00   1.00   20.00    --  103.00 -30.00 -60.00   61
  8  \w     34.00 128.00   1.00   20.00    --  103.00 -61.00   0.00   94
  9  \w     19.00 113.00   1.00    5.00    --   43.31  57.00 150.00   94
 10  \w     13.00 115.00   1.00    5.00    --   43.31  77.00  30.00  102
 11  \w     67.00 178.00   1.00   20.00    --  103.00  15.00 -60.00  111
 12  \w     67.00 178.00   1.00   20.00    --  103.00  15.00-180.00  111
 13  \w     80.00 176.00   1.00   20.00    --  103.00  30.00  60.00   96
 14  \w     22.00 109.00   1.00   20.00    --  103.00 -94.00-180.00   87
 15  \w    -96.00  -2.00   1.00    5.00    --  -43.31 125.00 -90.00   94
 16  \w     13.00 115.00   1.00    5.00    --   43.31  77.00-120.00  102
 17  \w     80.00 172.00   1.00   20.00    --  103.00  45.00   0.00   92
 18  \w     31.00 103.00   1.00   20.00    --  103.00-125.00  30.00   72
 19  \w     78.00 172.00   1.00   20.00    --  103.00  61.00-150.00   94
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_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      -0.1126995000
_diffrn_orient_matrix_UB_12      -0.0932795000
_diffrn_orient_matrix_UB_13      -0.0017590000
_diffrn_orient_matrix_UB_21      -0.0232892000
_diffrn_orient_matrix_UB_22      0.0202326000
_diffrn_orient_matrix_UB_23      0.0489907000
_diffrn_orient_matrix_UB_31      -0.0904907000
_diffrn_orient_matrix_UB_32      0.1109794000
_diffrn_orient_matrix_UB_33      -0.0104342000
_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_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            37850
_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         73.833
_diffrn_reflns_theta_min         4.201
_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    3.359
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.512
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6818
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0766P)^2^+0.4323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                6732
_reflns_number_total             6818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy02086d2.cif
_cod_data_source_block           mnhrsn
_cod_depositor_comments          'Adding full bibliography for 1548132.cif.'
_cod_original_cell_volume        3404.19(7)
_cod_database_code               1548132
_nottingham_internal_coll_name   MNHRSN
_nottingham_internal_coll_number 16826
_nottingham_internal_coll_client HRS/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '20.00, 5.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxhrs
_nottingham_internal_coll_date   19/01/2017
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 20/01/2017
_nottingham_internal_process_user pcxhrs
_nottingham_internal_solution_date 13/03/2017
_nottingham_internal_solution_user pcxhrs
_nottingham_internal_refinement_date 13/03/2017
_nottingham_internal_refinement_user pcxhrs
_nottingham_internal_self_archive_date 13/03/2017
_nottingham_internal_self_validation_date 13/03/2017
_nottingham_internal_self_validation_user pcxhrs
_nottingham_internal_validation_date 26/4/2017
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 26/4/2017
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C44 H42 Mn'
_chemical_oxdiff_usercomment
'MNHRSN #16826 GVA-1162 IN FOLMBIN FILM ON MICROMOUNT FOR HRS/DLK'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19), C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39),
  C40(H40), C41(H41)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C)
;
_shelx_res_checksum              48200
_olex2_date_sample_data_collection 2017-01-20
_olex2_date_sample_submission    2017-01-19
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id HS514
_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 1.500
_oxdiff_exptl_absorpt_empirical_full_min 0.683