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_7710750
_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         'C30 H40 Mg2 N4 O2 S4 Si2'
_chemical_formula_sum            'C30 H40 Mg2 N4 O2 S4 Si2'
_chemical_formula_weight         721.70
_chemical_name_systematic
'Magnesium bis(2-thiopyridyl)methylmethanide trimethylsiloxide'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-02-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6324(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.12561(18)
_cell_length_b                   9.98641(13)
_cell_length_c                   13.71565(17)
_cell_measurement_reflns_used    7202
_cell_measurement_temperature    100.03(11)
_cell_measurement_theta_max      75.1050
_cell_measurement_theta_min      4.4750
_cell_volume                     1791.94(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_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    -28.00  24.00   1.00    1.00    --  -44.33 -10.00-106.00   52
  2  \w    -79.00 -44.00   1.00    1.00    --  -44.33 -10.00-106.00   35
  3  \w   -128.00 -95.00   1.00    1.00    --  -44.33  10.00  66.00   33
  4  \w   -197.00 -63.00   1.00    1.00    -- -107.20 -10.00-106.00  134
  5  \w    -24.00  93.00   1.00    1.00    --    5.00  57.00-180.00  117
  6  \w    -76.00  45.00   1.00    1.00    --  -44.33  57.00 120.00  121
  7  \w    -91.00 -64.00   1.00    1.00    -- -107.20  76.00 -60.00   27
  8  \w    -61.00 -35.00   1.00    1.00    -- -107.20  57.00 -90.00   26
  9  \w   -117.00 -90.00   1.00    1.00    -- -107.20  76.00-120.00   27
 10  \w   -148.00 -20.00   1.00    1.00    -- -107.20  76.00-150.00  128
 11  \w    -64.00 -19.00   1.00    1.00    -- -107.20  57.00-150.00   45
 12  \w   -101.00 -72.00   1.00    1.00    -- -107.20  57.00-150.00   29
 13  \w   -139.00 -35.00   1.00    1.00    -- -107.20  57.00   0.00  104
 14  \w   -139.00-101.00   1.00    1.00    -- -107.20  57.00 -90.00   38
 15  \w   -123.00 -96.00   1.00    1.00    -- -107.20  76.00 -60.00   27
 16  \w    -70.00 -20.00   1.00    1.00    -- -107.20  10.00  66.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1144592000
_diffrn_orient_matrix_UB_12      0.0201218000
_diffrn_orient_matrix_UB_13      -0.0128995000
_diffrn_orient_matrix_UB_21      0.0236796000
_diffrn_orient_matrix_UB_22      -0.0071788000
_diffrn_orient_matrix_UB_23      0.1116485000
_diffrn_orient_matrix_UB_31      0.0140146000
_diffrn_orient_matrix_UB_32      -0.1529275000
_diffrn_orient_matrix_UB_33      -0.0070877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10871
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.571
_diffrn_reflns_theta_min         4.485
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_preparation       'Coated in Fomblin oil'
_exptl_crystal_recrystallization_method 'Crystallised from diethyl ether'
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0388P)^2^+1.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3337
_reflns_number_total             3609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02012b2.cif
_cod_data_source_block           2
_cod_database_code               7710750
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H40 Mg2 N4 O2 S4 Si2'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              52923
_olex2_exptl_crystal_mounting_method 'Mounted on a glass loop'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.848