Formation of a hydride containing amido-zincate using pinacolborane
Uzelac, Marina; Yuan, Kang; Nichol, Gary Stephen; Ingleson, Michael James; Dalton Transactions  (2021) –; doi:10.1039/D1DT02580E

data_7708332
_publ_section_title
;
 Formation of a hydride containing amido-zincate using pinacolborane
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02580E
_journal_year                    2021
_chemical_formula_moiety         '2(C40 H46 Li N3 O3 Zn)'
_chemical_formula_sum            'C80 H92 Li2 N6 O6 Zn2'
_chemical_formula_weight         1378.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.88420(10)
_cell_length_b                   14.3691(2)
_cell_length_c                   14.33240(10)
_cell_measurement_reflns_used    39147
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.6480
_cell_measurement_theta_min      4.3290
_cell_volume                     1805.79(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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   -116.00 -19.00   1.00    2.50    --  -41.67 -32.00 -58.00   97
  2  \w     19.00 116.00   1.00    2.50    --   41.67  32.00 100.00   97
  3  \w     88.00 178.00   1.00    7.50    --  111.00  32.00 100.00   90
  4  \w     37.00 134.00   1.00    7.50    --  111.00 -32.00 -58.00   97
  5  \w   -112.00 -15.00   1.00    2.50    --  -41.67 -57.00-120.00   97
  6  \w    -65.00  32.00   1.00    2.50    --  -41.67  32.00 100.00   97
  7  \w      5.00 120.00   1.00    2.50    --   41.67  19.00  60.00  115
  8  \w     61.00 128.00   1.00    2.50    --   41.67 178.00 120.00   67
  9  \w     61.00 128.00   1.00    2.50    --   41.67 178.00 -60.00   67
 10  \w     11.00  42.00   1.00    2.50    --   41.67  76.00 138.08   31
 11  \w     10.00  42.00   1.00    2.50    --   41.67  78.00  46.38   32
 12  \w    -32.00  65.00   1.00    2.50    --   41.67 -32.00 -58.00   97
 13  \w     14.00  42.00   1.00    2.50    --   46.00  80.00 -58.55   28
 14  \w     14.00  42.00   1.00    2.50    --   46.00  80.00 170.18   28
 15  \w     14.00  42.00   1.00    2.50    --   46.00  80.00-150.83   28
 16  \w     13.00  42.00   1.00    2.50    --   46.00  82.00  67.86   29
 17  \w     32.00 134.00   1.00    2.50    --   62.00  73.00  88.47  102
 18  \w     31.00 135.00   1.00    2.50    --   62.00  74.00 -14.63  104
 19  \w     31.00 135.00   1.00    2.50    --   62.00  74.00-121.50  104
 20  \w     31.00 135.00   1.00    2.50    --   62.00  74.00 166.96  104
 21  \w     35.00 139.00   1.00    2.50    --   66.00  74.00 -91.28  104
 22  \w     35.00 139.00   1.00    2.50    --   66.00  74.00 112.21  104
 23  \w     35.00 139.00   1.00    2.50    --   66.00  74.00 -49.16  104
 24  \w     36.00 138.00   1.00    2.50    --   66.00  73.00-168.34  102
 25  \w     40.00 142.00   1.00    2.50    --   70.00  72.00  37.29  102
 26  \w     40.00 142.00   1.00    2.50    --   70.00  72.00-119.50  102
 27  \w     39.00 143.00   1.00    2.50    --   70.00  74.00   9.82  104
 28  \w     46.00 144.00   1.00    2.50    --   74.00  61.00 -19.13   98
 29  \w     46.00 144.00   1.00    2.50    --   74.00  62.00 158.59   98
 30  \w     56.00  82.00   1.00    7.50    --   82.00  62.00  25.89   26
 31  \w     56.00  84.00   1.00    7.50    --   82.00  57.00  61.69   28
 32  \w     59.00  88.00   1.00    7.50    --   86.00  59.00 -80.75   29
 33  \w     60.00 100.00   1.00    7.50    --   86.00  65.00 110.04   40
 34  \w    112.00 162.00   1.00    7.50    --   90.00  72.00  71.33   50
 35  \w     60.00  89.00   1.00    7.50    --   90.00  72.00  71.33   29
 36  \w    134.00 159.00   1.00    7.50    --   90.00  57.00-125.67   25
 37  \w     64.00 127.00   1.00    7.50    --   90.00  57.00-125.67   63
 38  \w     61.00 130.00   1.00    7.50    --   90.00  72.00 176.15   69
 39  \w     65.00 152.00   1.00    7.50    --   94.00  71.00 -90.35   87
 40  \w     66.00  91.00   1.00    7.50    --   94.00  67.00 -19.84   25
 41  \w     76.00 102.00   1.00    7.50    --  106.00  71.00 -60.40   26
 42  \w     84.00 178.00   1.00    7.50    --  111.00  61.00-180.00   94
 43  \w     31.00 106.00   1.00    7.50    --  111.00 -94.00   0.00   75
 44  \w     41.00 112.00   1.00    7.50    --  111.00-125.00 150.00   71
 45  \w    135.00 168.00   1.00    7.50    --  111.00  70.00 125.34   33
 46  \w     75.00 112.00   1.00    7.50    --  111.00-125.00 -60.00   37
 47  \w     81.00 130.00   1.00    7.50    --  111.00  70.00 125.34   49
 48  \w    127.00 178.00   1.00    7.50    --  111.00  61.00   0.00   51
 49  \w     84.00 113.00   1.00    7.50    --  111.00  61.00   0.00   29
 50  \w     31.00 107.00   1.00    7.50    --  111.00 -94.00 150.00   76
 51  \w     88.00 119.00   1.00    7.50    --  111.00  61.00 -90.00   31
 52  \w     78.00 108.00   1.00    7.50    --  111.00-102.00  71.11   30
 53  \w     45.00 120.00   1.00    7.50    --  111.00 -45.00 150.00   75
 54  \w     62.00 136.00   1.00    7.50    --  111.00 -61.00 -30.00   74
 55  \w     84.00 162.00   1.00    7.50    --  111.00  61.00  60.00   78
 56  \w     83.00 128.00   1.00    7.50    --  111.00  61.00  90.00   45
 57  \w    111.00 176.00   1.00    7.50    --  111.00  61.00-150.00   65
 58  \w     83.00 110.00   1.00    7.50    --  111.00  61.00-150.00   27
 59  \w     83.00 132.00   1.00    7.50    --  111.00  61.00  30.00   49
 60  \w    129.00 168.00   1.00    7.50    --  111.00  63.00 -20.48   39
 61  \w     84.00 123.00   1.00    7.50    --  111.00  63.00 -20.48   39
 62  \w    130.00 157.00   1.00    7.50    --  111.00  61.00 120.00   27
 63  \w     83.00 173.00   1.00    7.50    --  111.00  61.00 150.00   90
 64  \w     87.00 129.00   1.00    7.50    --  111.00  45.00 -90.00   42
 65  \w     66.00 107.00   1.00    7.50    --  111.00 -94.00-150.00   41
 66  \w     83.00 109.00   1.00    7.50    --  111.00  61.00 120.00   26
 67  \w     31.00 107.00   1.00    7.50    --  111.00 -94.00 -60.00   76
 68  \w    129.00 178.00   1.00    7.50    --  111.00  55.00-124.68   49
 69  \w     85.00 112.00   1.00    7.50    --  111.00  55.00-124.68   27
 70  \w     53.00  93.00   1.00    7.50    --  111.00-125.00-150.00   40
 71  \w    142.00 172.00   1.00    7.50    --  111.00  45.00 -90.00   30
 72  \w     82.00 109.00   1.00    7.50    --  111.00  67.00  33.35   27
 73  \w    125.00 170.00   1.00    7.50    --  111.00  67.00  33.35   45
 74  \w    112.00 157.00   1.00    7.50    --  111.00  61.00 -30.00   45
 75  \w     84.00 109.00   1.00    7.50    --  111.00  61.00 -30.00   25
 76  \w     84.00 177.00   1.00    7.50    --  111.00  61.00 -60.00   93
 77  \w     31.00 103.00   1.00    7.50    --  111.00 -94.00 -30.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0245244000
_diffrn_orient_matrix_UB_12      -0.0409739000
_diffrn_orient_matrix_UB_13      -0.0956493000
_diffrn_orient_matrix_UB_21      -0.1729523000
_diffrn_orient_matrix_UB_22      -0.0164445000
_diffrn_orient_matrix_UB_23      -0.0265177000
_diffrn_orient_matrix_UB_31      -0.0185815000
_diffrn_orient_matrix_UB_32      0.0977442000
_diffrn_orient_matrix_UB_33      -0.0447509000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54236
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.206
_diffrn_reflns_theta_min         4.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.6234
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0930 after correction.
The Ratio of minimum to maximum transmission is 0.8268.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       blade
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of THF and hexane  by solvent layering'
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7357
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0907P)^2^+0.3772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                7110
_reflns_number_total             7357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02580e2.cif
_cod_data_source_block           mi20022
_cod_database_code               7708332
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C80 H88 Li2 N6 O6 Zn2 '
_chemical_oxdiff_usercomment     '@ 120 K MU420'
_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. Others
 Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32C)=
 Sof(H32D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C30(H30C,H30D), C31(H31A,H31B), C31A(H31C,
 H31D), C32(H32A,H32B), C32A(H32C,H32D), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C17(H17), C18(H18), C23(H23), C24(H24), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              28226
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 4.436
_oxdiff_exptl_absorpt_empirical_full_min 0.352