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_7710751
_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         'C22 H18 Mg N4 S4, C24 H20 P2'
_chemical_formula_sum            'C46 H38 Mg N4 P2 S4'
_chemical_formula_weight         861.29
_chemical_name_systematic
'Magnesium bis(2-thiopyridyl)methanide tetraphenyldiphosphine'
_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 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 108.2140(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.69497(18)
_cell_length_b                   16.4661(3)
_cell_length_c                   13.4773(2)
_cell_measurement_reflns_used    7927
_cell_measurement_temperature    100.02(14)
_cell_measurement_theta_max      74.9400
_cell_measurement_theta_min      4.3630
_cell_volume                     2043.69(7)
_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      100.02(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_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      7.00  32.00   1.00    1.00    --    5.00  44.00 -76.00   25
  2  \w    -46.00 -21.00   1.00    1.00    --    5.00 -44.00 132.00   25
  3  \w    -95.00 -70.00   1.00    1.00    --  -44.33 -44.00 132.00   25
  4  \w    -76.00  44.00   1.00    1.00    --  -44.33  44.00 -76.00  120
  5  \w   -106.00 -49.00   1.00    1.00    --  -46.47 -44.00 132.00   57
  6  \w   -144.00 -20.00   1.00    1.00    -- -107.20  44.00 -76.00  124
  7  \w   -174.00-149.00   1.00    1.00    -- -107.20 -44.00 132.00   25
  8  \w   -133.00 -11.00   1.00    1.00    --  -44.33 -57.00  30.00  122
  9  \w    -36.00 -10.00   1.00    1.00    --  -46.47  57.00   0.00   26
 10  \w   -139.00-113.00   1.00    1.00    -- -107.20 -76.00-120.00   26
 11  \w   -197.00 -18.00   1.00    1.00    -- -107.20  19.00 150.00  179
 12  \w   -107.00 -69.00   1.00    1.00    -- -107.20  57.00 120.00   38
 13  \w    -55.00 -19.00   1.00    1.00    -- -107.20  57.00 120.00   36
 14  \w   -121.00 -94.00   1.00    1.00    -- -107.20  38.00-120.00   27
 15  \w   -190.00-163.00   1.00    1.00    -- -107.20 -76.00-120.00   27
 16  \w    -60.00 -18.00   1.00    1.00    -- -107.20  38.00-120.00   42
 17  \w   -138.00 -35.00   1.00    1.00    -- -107.20  38.00 120.00  103
;
_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      -0.0209449000
_diffrn_orient_matrix_UB_12      -0.0460323000
_diffrn_orient_matrix_UB_13      0.0937258000
_diffrn_orient_matrix_UB_21      -0.1543561000
_diffrn_orient_matrix_UB_22      -0.0244253000
_diffrn_orient_matrix_UB_23      -0.0671543000
_diffrn_orient_matrix_UB_31      0.0609714000
_diffrn_orient_matrix_UB_32      -0.0777246000
_diffrn_orient_matrix_UB_33      -0.0344584000
_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  0.0196
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.907
_diffrn_reflns_theta_min         4.375
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.809
_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            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       irregular
_exptl_crystal_F_000             896
_exptl_crystal_preparation       'Coated in Fomblin oil'
_exptl_crystal_recrystallization_method 'Crystallised from toluene'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0380P)^2^+1.6169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3834
_reflns_number_total             4131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02012b2.cif
_cod_data_source_block           6
_cod_original_cell_volume        2043.69(6)
_cod_database_code               7710751
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mg C46 P2 N4 S4'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23)
;
_shelx_res_checksum              18367
_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 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.883