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_7708336
_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         'C34 H42 Li N3 O3 Zn'
_chemical_formula_sum            'C34 H42 Li N3 O3 Zn'
_chemical_formula_weight         613.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-12
_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                 106.863(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3465(5)
_cell_length_b                   15.5769(6)
_cell_length_c                   18.7091(9)
_cell_measurement_reflns_used    17426
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      29.6280
_cell_measurement_theta_min      3.5790
_cell_volume                     3164.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.921
_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    -91.00 -27.00   1.00   22.50    --  -18.82 164.00 145.00   64
  2  \w    -67.00   7.00   1.00   22.50    --  -18.82 116.00  -2.00   74
  3  \w     -7.00  69.00   1.00   22.50    --   20.54-116.00 -91.00   76
  4  \w     27.00  93.00   1.00   22.50    --   20.54-164.00 120.00   66
  5  \w    -39.00   8.00   1.00   22.50    --  -18.82 -77.00 120.00   47
  6  \w    -91.00 -39.00   1.00   22.50    --  -18.82-178.00 -60.00   52
  7  \w    -88.00   0.00   1.00   22.50    --  -18.82 -37.00 -30.00   88
  8  \w    -38.00  50.00   1.00   22.50    --  -18.82  37.00 150.00   88
  9  \w    -36.00  48.00   1.00   22.50    --  -18.82  57.00 -90.00   84
 10  \w     39.00  93.00   1.00   22.50    --   20.54 178.00 -30.00   54
 11  \w     -6.00  39.00   1.00   22.50    --   20.54  77.00   0.00   45
 12  \w     -6.00  39.00   1.00   22.50    --   20.54  77.00 120.00   45
 13  \w     -6.00  39.00   1.00   22.50    --   20.54  77.00  60.00   45
 14  \w     -6.00  39.00   1.00   22.50    --   20.54  77.00 -60.00   45
 15  \w    -49.00  40.00   1.00   22.50    --   20.54 -37.00 -90.00   89
 16  \w     -9.00  92.00   1.00   22.50    --   20.54  19.00-120.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0160154000
_diffrn_orient_matrix_UB_12      0.0336837000
_diffrn_orient_matrix_UB_13      0.0266041000
_diffrn_orient_matrix_UB_21      0.0021200000
_diffrn_orient_matrix_UB_22      0.0291805000
_diffrn_orient_matrix_UB_23      -0.0287164000
_diffrn_orient_matrix_UB_31      -0.0632537000
_diffrn_orient_matrix_UB_32      0.0094681000
_diffrn_orient_matrix_UB_33      -0.0060879000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78720
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.724
_diffrn_reflns_theta_min         3.343
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.287
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         9075
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0433P)^2^+2.2418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6396
_reflns_number_total             9075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02580e2.cif
_cod_data_source_block           mu384_reproces
_cod_database_code               7708336
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 Li1 N3 O3 C34 H42'
_chemical_oxdiff_usercomment     '120 K colourless cube'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 C34, C33, C32, C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
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), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22)
;
_shelx_res_checksum              18769
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.811