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_7063103
_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 Cl2 Mg2 N8 O, 0.2[C7H8]'
_chemical_formula_sum            'C41.4 H51.6 Cl2 Mg2 N8 O'
_chemical_formula_weight         796.82
_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   mixed
_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                 95.8020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4870(4)
_cell_length_b                   13.7899(7)
_cell_length_c                   31.3556(14)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.529
_cell_measurement_theta_min      2.453
_cell_volume                     4081.1(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      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.1191
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            56313
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.407
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1501 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.6105.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8294
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0412P)^2^+5.5485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5590
_reflns_number_total             8294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00492b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7063101--7063105.cif.'
_cod_original_formula_sum        'C41.40 H51.60 Cl2 Mg2 N8 O'
_cod_database_code               7063103
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.991
_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
 C40-C39 \\sim C40-C39A
 with sigma of 0.02
 C38A-C37 \\sim C38-C37
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C40 \\sim C37 \\sim C39 \\sim C38 \\sim C39A \\sim C38A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C39A, C38A, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C39, C38, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(H40C)=Sof(H40D)=Sof(H37C)=Sof(H37D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
 Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(H40A)=Sof(H40B)=Sof(H37A)=Sof(H37B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C33(H33A,H33B), C34(H34A,H34B), C28(H28A,H28B), C16(H16A,
 H16B), C10(H10A,H10B), C40(H40A,H40B), C40(H40C,H40D), C37(H37A,H37B),
 C37(H37C,H37D), C39(H39A,H39B), C38(H38A,H38B), C39A(H39C,H39D), C38A(H38C,
 H38D)
6.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C23(H23), C27(H27), C14(H14), C9(H9), C12(H12), C22(H22), C13(H13),
 C21(H21), C20(H20), C2(H2), C3(H3), C32(H32), C5(H5), C30(H30), C4(H4),
 C31(H31)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 42 electrons were 
found in a volume of 234\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.2[C6H14] per Asymmetric Unit 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66886
_shelx_fab_checksum              68235
_olex2_submission_special_instructions 'No special instructions were received'