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_7063102
_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         'C30 H45 Br Mg N4 O3'
_chemical_formula_sum            'C30 H45 Br Mg N4 O3'
_chemical_formula_weight         613.92
_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             2024-03-07
_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                 113.6190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0348(7)
_cell_length_b                   10.8915(4)
_cell_length_c                   17.4378(6)
_cell_measurement_reflns_used    8952
_cell_measurement_temperature    223.0
_cell_measurement_theta_max      24.464
_cell_measurement_theta_min      2.240
_cell_volume                     3138.3(2)
_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      223.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0933
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32043
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.263
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1033 before and 0.0774 after correction.
The Ratio of minimum to maximum transmission is 0.8439.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0487
_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^)+(0.1000P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3586
_reflns_number_total             5733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00492b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7063101--7063105.cif.'
_cod_database_code               7063102
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.772
_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
 C19-C20A \\sim C20A-C20
 with sigma of 0.02
 C20A-C21A \\sim C20-C21
 with sigma of 0.02
 C21A-C20A \\sim C20-C21
 with sigma of 0.02
 C21A-C22 \\sim C22-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C20A) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H22C)=Sof(H22D)=Sof(H19C)=Sof(H19D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=
 Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(H19A)=Sof(H19B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C10(H10A,H10B), C16(H16A,H16B), C30(H30A,H30B), C22(H22A,
 H22B), C22(H22C,H22D), C23(H23A,H23B), C19(H19A,H19B), C19(H19C,H19D),
 C26(H26A,H26B), C27(H27A,H27B), C24(H24A,H24B), C29(H29A,H29B), C28(H28A,H28B),
  C25(H25A,H25B), C21(H21A,H21B), C20(H20A,H20B), C21A(H21C,H21D), C20A(H20C,
 H20D)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C5(H5), C3(H3), C14(H14), C7(H7), C4(H4), C12(H12), C13(H13)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              63717
_olex2_submission_special_instructions 'No special instructions were received'