Magnesium(ii) complexes supported by indole- and pyrrole-containing Schiff-base ligands: syntheses, structures, and applications as precatalysts in the hydroboration of nitriles and alkynes
Wu, Mengxiang; Chen, Ling; Yang, Xiaohan; Li, Yahong; New Journal of Chemistry 48 (2024) 7125–7133; doi:10.1039/D4NJ00492B

data_7063105
_publ_section_title
;
 Magnesium(ii) complexes supported by indole- and pyrrole-containing
 Schiff-base ligands: syntheses, structures, and applications as
 precatalysts in the hydroboration of nitriles and alkynes
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7125
_journal_page_last               7133
_journal_paper_doi               10.1039/D4NJ00492B
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C40 H50 Br1.854 Mg2 N8 O'
_chemical_formula_sum            'C40 H50 Br1.86 Mg2 N8 O'
_chemical_formula_weight         855.73
_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             2024-03-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4766(4)
_cell_length_b                   13.9573(5)
_cell_length_c                   31.4956(11)
_cell_measurement_reflns_used    9190
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      2.44
_cell_volume                     4143.3(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SMART APEX II diffractometer'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            117735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.533
_diffrn_reflns_theta_min         2.608
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.888
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1067 before and 0.0908 after correction.
The Ratio of minimum to maximum transmission is 0.7230.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8523
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+3.3867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6813
_reflns_number_total             8523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00492b2.cif
_cod_data_source_block           4-2
_cod_depositor_comments
'Adding full bibliography for 7063101--7063105.cif.'
_cod_database_code               7063105
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C38 \\sim C37-C41
 with sigma of 0.02
 C38-C39 \\sim C41-C01I
 with sigma of 0.02
 C41-C01I \\sim C39-C38
 with sigma of 0.01
 C40-C39 \\sim C40-C01I
 with sigma of 0.02
 C41-C37 \\sim C38-C37
 with sigma of 0.01
 C01I-C40 \\sim C39-C40
 with sigma of 0.01
 C37-C39 \\sim C37-C01I
 with sigma of 0.04
 C38-C40 \\sim C41-C40
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H37A(0.85) H37B(0.85) H37C(0.15) H37D(0.15) C38(0.85) H38A(0.85)
 H38B(0.85) H40A(0.7) H40B(0.7) H40C(0.3) H40D(0.3) C39(0.7) H39A(0.7)
 H39B(0.7) C41(0.15) H41A(0.15) H41B(0.15) C01I(0.3) H01A(0.3) H01B(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C15(H15A,H15B), C16(H16A,H16B), C33(H33A,H33B), C28(H28A,
 H28B), C10(H10A,H10B), C37(H37A,H37B), C37(H37C,H37D), C38(H38A,H38B),
 C40(H40A,H40B), C40(H40C,H40D), C39(H39A,H39B), C41(H41A,H41B), C01I(H01A,H01B)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C20(H20), C7(H7), C9(H9), C21(H21), C30(H30), C22(H22), C32(H32),
 C5(H5), C2(H2), C25(H25), C14(H14), C31(H31), C23(H23), C3(H3), C12(H12),
 C13(H13), C4(H4)
5.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              10205
_olex2_submission_special_instructions 'No special instructions were received'