Solvent-free Zn (NSNO) complex-catalysed dihydroboration of nitriles
Ataie, Saeed; Ovens, Jeffrey S.; Tom Baker, R.; Chemical Communications  (2022) –; doi:10.1039/D2CC03517K

data_7130324
_publ_section_title
;
 Solvent-free Zn (NSNO) complex-catalysed dihydroboration of nitriles
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03517K
_journal_year                    2022
_chemical_formula_moiety         'C38 H32 N4 O2 S2 Zn2, 4(C4 H8 O)'
_chemical_formula_sum            'C54 H64 N4 O6 S2 Zn2'
_chemical_formula_weight         1059.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                88.174(2)
_cell_angle_beta                 83.185(2)
_cell_angle_gamma                80.990(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9532(13)
_cell_length_b                   10.9777(14)
_cell_length_c                   12.1123(16)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.51
_cell_volume                     1297.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
; 
 SHELXT 2014/5 (Sheldrick, 2014)
;
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31432
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.665
_diffrn_reflns_theta_min         1.693
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8030
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0852P)^2^+0.2735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5376
_reflns_number_total             8030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03517k2.cif
_cod_data_source_block           K0572
_cod_database_code               7130324
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              1090
_shelx_hkl_checksum              95755