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_7708334
_publ_section_title
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 Formation of a hydride containing amido-zincate using pinacolborane
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02580E
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H32 B2 Li2 N6 O2'
_chemical_formula_sum            'C26 H32 B2 Li2 N6 O2'
_chemical_formula_weight         496.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-07
_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            4
_cell_length_a                   10.756(3)
_cell_length_b                   15.008(4)
_cell_length_c                   17.229(5)
_cell_measurement_reflns_used    1920
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      20.02
_cell_measurement_theta_min      2.29
_cell_volume                     2781.2(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Diamond Light Souce Beamline I-19'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18741
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        18.244
_diffrn_reflns_theta_max         18.244
_diffrn_reflns_theta_min         1.744
_diffrn_source                   Synchrotron
_diffrn_source_current           0.0
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_power             0.0
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_entry.id                        xia2
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.5192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1246 before and 0.0741 after correction.
The Ratio of minimum to maximum transmission is 0.6974.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 533 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         2181
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0606P)^2^+0.9261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.711
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1597
_reflns_number_total             2181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02580e2.cif
_cod_data_source_block           mi21006
_cod_database_code               7708334
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.997
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H,H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B2-H2B = B2-H2D = B2-H2C = B2-H2A
 1.16 with sigma of 0.02
 H2D-H2C
 1.86 with sigma of 0.04
 H2A-H2C
 1.86 with sigma of 0.04
 H2B-H2D
 1.86 with sigma of 0.04
 H2D-H2A
 1.86 with sigma of 0.04
 H2B-H2A
 1.86 with sigma of 0.04
 H2B-H2C
 1.86 with sigma of 0.04
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a 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), C17(H17), C24(H24), C25(H25), C26(H26)
4.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              23647
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'