Synthesis, Characterisation and Reactivity of Group 2 Complexes with a Thiopyridyl Scorpionate Ligand
Stevens, Matthew Philip; Spray, Emily; Vitorica-Yrzebal, Inigo; Singh, Kuldip; Timmermann, Vanessa M.; Sotorrios, Lia; Macgregor, Stuart Alan; Ortu, Fabrizio; Dalton Transactions  (2022) –; doi:10.1039/D2DT02012B

data_7710756
_publ_section_title
;
 Synthesis, Characterisation and Reactivity of Group 2 Complexes with a
 Thiopyridyl Scorpionate Ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02012B
_journal_year                    2022
_chemical_formula_moiety         '2(C20 H21 Mg N3 S3)'
_chemical_formula_sum            'C40 H42 Mg2 N6 S6'
_chemical_formula_weight         847.77
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                87.806(5)
_cell_angle_beta                 76.581(5)
_cell_angle_gamma                79.929(5)
_cell_formula_units_Z            2
_cell_length_a                   12.1983(6)
_cell_length_b                   12.2683(8)
_cell_length_c                   14.8689(10)
_cell_measurement_reflns_used    2589
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      27.1430
_cell_measurement_theta_min      3.6340
_cell_volume                     2131.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      99.9(2)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -83.00  -7.00   1.00   10.00    --  -18.04 -57.00 -30.00   76
  2  \w     63.00  94.00   1.00   10.00    --   19.45 178.00-150.00   31
  3  \w    -11.00  25.00   1.00   10.00    --   19.45  77.00 -30.00   36
  4  \w    -37.00  47.00   1.00   10.00    --   19.45 -77.00-150.00   84
  5  \w     -7.00  22.00   1.00   10.00    --   19.45  77.00-180.00   29
  6  \w     -3.00  42.00   1.00   10.00    --   19.45  77.00  60.00   45
  7  \w    -54.00  72.00   1.00   10.00    --   19.45   0.00-150.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.1332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18611
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.114
_diffrn_reflns_theta_min         3.373
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99635
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0749
_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^)+(0.0264P)^2^+0.5729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6209
_reflns_number_total             9751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02012b2.cif
_cod_data_source_block           1
_cod_database_code               7710756
_shelx_shelxl_version_number     2018/3
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              22848
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;