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_7063101
_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 Cl Mg N4 O3'
_chemical_formula_sum            'C30 H45 Cl Mg N4 O3'
_chemical_formula_weight         569.46
_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             2024-03-06
_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                 113.5430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8805(6)
_cell_length_b                   10.8261(4)
_cell_length_c                   17.4012(6)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    223.0
_cell_measurement_theta_max      26.326
_cell_measurement_theta_min      2.255
_cell_volume                     3088.07(19)
_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 0.998
_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  0.0816
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39925
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.274
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1467 before and 0.0887 after correction.
The Ratio of minimum to maximum transmission is 0.8998.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7071
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.0817
_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^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3656
_reflns_number_total             7071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00492b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7063101--7063105.cif.'
_cod_database_code               7063101
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C27 \\sim C27-C31
 with sigma of 0.02
 C31-C0 \\sim C27-C28
 with sigma of 0.02
 O3-C31 \\sim C31-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C00{) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C0) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(C00{)=Sof(H00A)=Sof(H00B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C0)=Sof(H0A)=
 Sof(H0B)=Sof(C32)=Sof(H32A)=Sof(H32B)=1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C28)=Sof(H28A)=
 Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C15(H15A,H15B), C22(H22A,H22B), C16(H16A,H16B), C23(H23A,
 H23B), C26(H26A,H26B), C27(H27A,H27B), C21(H21A,H21B), C20(H20A,H20B),
 C19(H19A,H19B), C30(H30A,H30B), C25(H25A,H25B), C24(H24A,H24B), C28(H28A,H28B),
  C29(H29A,H29B), C00{(H00A,H00B), C31(H31A,H31B), C0(H0A,H0B), C32(H32A,H32B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C14(H14), C3(H3), C2(H2), C12(H12), C7(H7), C5(H5), C4(H4), C13(H13)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              72591
_olex2_submission_special_instructions 'No special instructions were received'