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_7708337
_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         'C23 H21 N3 Zn'
_chemical_formula_sum            'C23 H21 N3 Zn'
_chemical_formula_weight         404.80
_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             2021-02-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.724(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8368(2)
_cell_length_b                   14.6402(2)
_cell_length_c                   14.2478(2)
_cell_measurement_reflns_used    17179
_cell_measurement_temperature    120.01(13)
_cell_measurement_theta_max      29.0610
_cell_measurement_theta_min      3.9980
_cell_volume                     1975.08(6)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.907
_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    -35.00  54.00   1.00   20.00    --  -15.82  36.00  50.00   89
  2  \w    -85.00   4.00   1.00   20.00    --  -15.82 -36.00-106.00   89
  3  \w     -2.00  87.00   1.00   20.00    --   17.54  36.00  50.00   89
  4  \w    -52.00  37.00   1.00   20.00    --   17.54 -36.00-106.00   89
  5  \w    -39.00  11.00   1.00   20.00    --  -15.82 -77.00 120.00   50
  6  \w     -9.00  39.00   1.00   20.00    --   17.54  77.00 -60.00   48
  7  \w    -20.00  56.00   1.00   20.00    --   17.54 -99.00-120.00   76
  8  \w    -20.00  56.00   1.00   20.00    --   17.54 -99.00  60.00   76
  9  \w      1.00  85.00   1.00   20.00    --   17.54  57.00 -30.00   84
 10  \w     39.00  90.00   1.00   20.00    --   17.54 178.00-150.00   51
 11  \w    -39.00  11.00   1.00   20.00    --  -15.82 -77.00-180.00   50
 12  \w    -39.00  11.00   1.00   20.00    --  -15.82 -77.00  60.00   50
 13  \w    -20.00  56.00   1.00   20.00    --   17.54 -99.00 -30.00   76
 14  \w    -20.00   7.00   1.00   20.00    --   17.54 -99.00 150.00   27
 15  \w     -9.00  39.00   1.00   20.00    --   17.54  77.00 120.00   48
;
_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      0.0329427000
_diffrn_orient_matrix_UB_12      -0.0195921000
_diffrn_orient_matrix_UB_13      0.0460855000
_diffrn_orient_matrix_UB_21      0.0672531000
_diffrn_orient_matrix_UB_22      0.0105935000
_diffrn_orient_matrix_UB_23      -0.0064297000
_diffrn_orient_matrix_UB_31      -0.0015514000
_diffrn_orient_matrix_UB_32      0.0430259000
_diffrn_orient_matrix_UB_33      0.0225901000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43196
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.415
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86852
_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    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_recrystallization_method
'The material was recrystallised by slow cooling of boiling 1,2-difluorobenzene solution to room temperature.'
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0131P)^2^+2.6340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4287
_reflns_number_total             4951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02580e2.cif
_cod_data_source_block           mu506_reprocess
_cod_database_code               7708337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H21 N3 Zn'
_chemical_oxdiff_usercomment     '120 K'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C22(H22), C8(H8), C12(H12), C21(H21), C19(H19), C6(H6), C17(H17), C2(H2),
 C9(H9), C20(H20), C14(H14), C11(H11), C10(H10), C16(H16), C15(H15), C3(H3),
 C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c)
;
_shelx_res_checksum              37678
_olex2_exptl_crystal_mounting_method
'The crystal was mountedon a MITIGEN holder in oil.'
_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 1.215
_oxdiff_exptl_absorpt_empirical_full_min 0.906