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_7708333
_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         'C30 H24 N9 Zn2, C12 H8 B O4, C6 H6 O2'
_chemical_formula_sum            'C48 H38 B N9 O6 Zn2'
_chemical_formula_weight         978.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0270(8)
_cell_length_b                   17.4139(7)
_cell_length_c                   8.5193(3)
_cell_measurement_reflns_used    5548
_cell_measurement_temperature    120.01(13)
_cell_measurement_theta_max      23.4420
_cell_measurement_theta_min      3.8020
_cell_volume                     2080.96(16)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -52.00  26.00   1.00   30.00    --  -16.31  93.00 -50.00   78
  2  \w    -10.00  20.00   1.00   30.00    --  -16.31 -93.00-162.00   30
  3  \w    -27.00  52.00   1.00   30.00    --   18.03 -93.00-162.00   79
  4  \w    -69.00 -40.00   1.00   30.00    --  -16.31-178.00 -30.00   29
  5  \w    -33.00   5.00   1.00   30.00    --  -16.31  57.00  60.00   38
  6  \w    -27.00   8.00   1.00   30.00    --  -16.31 -77.00  60.00   35
  7  \w    -32.00  46.00   1.00   30.00    --  -16.31  57.00  90.00   78
  8  \w     -3.00  46.00   1.00   30.00    --  -16.31  57.00-150.00   49
  9  \w    -10.00  15.00   1.00   30.00    --   18.03  77.00-180.00   25
 10  \w    -48.00  36.00   1.00   30.00    --   18.03 -57.00 -60.00   84
;
_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      -0.0016847000
_diffrn_orient_matrix_UB_12      -0.0488060000
_diffrn_orient_matrix_UB_13      -0.0105444000
_diffrn_orient_matrix_UB_21      -0.0327249000
_diffrn_orient_matrix_UB_22      0.0123934000
_diffrn_orient_matrix_UB_23      -0.0361160000
_diffrn_orient_matrix_UB_31      0.0765206000
_diffrn_orient_matrix_UB_32      0.0042351000
_diffrn_orient_matrix_UB_33      -0.0156980000
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19725
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         3.346
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81912
_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    1.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 1162 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0621P)^2^+2.0314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3194
_reflns_number_total             3800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02580e2.cif
_cod_data_source_block           mu528_reprocess
_cod_original_cell_volume        2080.97(16)
_cod_database_code               7708333
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 N3 B1 O4 C20 H30 '
_chemical_oxdiff_usercomment     '120 K'
_reflns_odcompleteness_completeness 99.55
_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 O(H) groups
2. Shared sites
{C16, C16A}
{C17, C17A}
{C18, C18A}
{C19, C19A}
{C20, C20A}
{C21, C21A}
{C22, C22A}
{C23, C23A}
3. Restrained distances
 O1-C16 \\sim O2-C17 \\sim O4-C23 \\sim O3-C22 \\sim O3-C22A
 with sigma of 0.02
 C25-C24 \\sim C24-C23A \\sim C23A-C22A
 with sigma of 0.02
 O4-C23 \\sim O3-C22A \\sim O1-C16 \\sim O2-C17
 with sigma of 0.02
 O3-B1 \\sim O2-B1 \\sim O1-B1 \\sim O4-B1
 with sigma of 0.02
4. Rigid bond restraints
 O3, O4, C22, C22A, C23, C23A, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim C22 \\sim C22A \\sim C23 \\sim C23A \\sim C24 \\sim C25:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
6. Rigid body (RIGU) restrains
 O3, O4, C22, C22A, C23, C23A, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: O1(0.5) O2(0.5) O4(0.5) C16(0.5) C17(0.5) C18(0.5) H18(0.5)
 C19(0.5) H19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C22(0.25) C22A(0.25)
 C23(0.5) C23A(0.5) H23A(0.5) B1(0.5) O5(0.5) H5(0.5) O6(0.5) H6(0.5) C16A(0.5)
 H16A(0.5) C17A(0.5) C18A(0.5) C19A(0.5) H19A(0.5) C20A(0.5) H20A(0.5)
 C21A(0.5) H21A(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C18(H18), C19(H19), C20(H20), C21(H21),
 C23A(H23A), C24(H24), C25(H25), C16A(H16A), C19A(H19A), C20A(H20A), C21A(H21A)
8.b Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6)
;
_shelx_res_checksum              70921
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.831