#------------------------------------------------------------------------------
#$Date: 2022-07-23 03:15:30 +0300 (Sat, 23 Jul 2022) $
#$Revision: 276839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/07/7710755.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710755
loop_
_publ_author_name
'Stevens, Matthew Philip'
'Spray, Emily'
'Vitorica-Yrzebal, Inigo'
'Singh, Kuldip'
'Timmermann, Vanessa M.'
'Sotorrios, Lia'
'Macgregor, Stuart Alan'
'Ortu, Fabrizio'
_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         'C14 H18 Mg N2 O2 S2'
_chemical_formula_sum            'C14 H18 Mg N2 O2 S2'
_chemical_formula_weight         334.73
_chemical_name_systematic        'Magnesium bis(2-thiopyridide) DME adduct'
_chemical_properties_physical    Air-sensitive,Moisture-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             2021-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.135(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6270(3)
_cell_length_b                   12.5306(5)
_cell_length_c                   14.0589(5)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      72.209
_cell_measurement_theta_min      3.527
_cell_volume                     1658.06(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23132
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.464
_diffrn_reflns_theta_min         4.775
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.323
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1522 before and 0.0951 after correction.
The Ratio of minimum to maximum transmission is 0.5413.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_preparation       'Coated in Fomblin oil'
_exptl_crystal_recrystallization_method 'Crystallised from DME'
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0365
_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/[σ²(Fo²)+(0.0433P)²+1.0832P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2872
_reflns_number_total             3267
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02012b2.cif
_cod_data_source_block           4-Mg
_cod_database_code               7710755
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.644
_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:
 C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_olex2_exptl_crystal_mounting_method 'Mounted on a glass loop'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.55411(5) 0.11845(4) 0.63514(4) 0.01981(13) Uani 1 1 d . . . . .
S2 S 0.08962(5) 0.29845(4) 0.65883(3) 0.02087(14) Uani 1 1 d . . . . .
Mg1 Mg 0.30480(6) 0.19607(5) 0.62165(4) 0.01443(15) Uani 1 1 d . . . . .
O1 O 0.19742(13) 0.05776(10) 0.55813(9) 0.0174(3) Uani 1 1 d . . . . .
O2 O 0.24804(13) 0.23858(10) 0.47137(9) 0.0178(3) Uani 1 1 d . . . . .
N1 N 0.46889(15) 0.31359(12) 0.65956(11) 0.0153(3) Uani 1 1 d . . . . .
N2 N 0.26900(16) 0.16477(12) 0.76382(11) 0.0170(3) Uani 1 1 d . . . . .
C1 C 0.58648(18) 0.25257(15) 0.66281(13) 0.0149(4) Uani 1 1 d . . . . .
C2 C 0.72298(19) 0.29855(16) 0.68701(14) 0.0200(4) Uani 1 1 d . . . . .
H2 H 0.804973 0.255934 0.688323 0.024 Uiso 1 1 calc R U . . .
C3 C 0.7366(2) 0.40529(17) 0.70864(14) 0.0229(4) Uani 1 1 d . . . . .
H3 H 0.828121 0.437032 0.724671 0.027 Uiso 1 1 calc R U . . .
C4 C 0.6150(2) 0.46743(16) 0.70704(15) 0.0229(4) Uani 1 1 d . . . . .
H4 H 0.622413 0.541223 0.722794 0.028 Uiso 1 1 calc R U . . .
C5 C 0.4842(2) 0.41817(15) 0.68189(14) 0.0192(4) Uani 1 1 d . . . . .
H5 H 0.401239 0.459796 0.680230 0.023 Uiso 1 1 calc R U . . .
C6 C 0.15320(19) 0.22644(15) 0.76420(14) 0.0183(4) Uani 1 1 d . . . . .
C7 C 0.0944(2) 0.23049(17) 0.84801(15) 0.0247(4) Uani 1 1 d . . . . .
H7 H 0.009814 0.269745 0.847412 0.030 Uiso 1 1 calc R U . . .
C8 C 0.1604(2) 0.17738(18) 0.93006(16) 0.0298(5) Uani 1 1 d . . . . .
H8 H 0.122554 0.180654 0.987197 0.036 Uiso 1 1 calc R U . . .
C9 C 0.2829(2) 0.11851(17) 0.92992(15) 0.0289(5) Uani 1 1 d . . . . .
H9 H 0.331590 0.083347 0.987137 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3320(2) 0.11246(16) 0.84462(15) 0.0230(4) Uani 1 1 d . . . . .
H10 H 0.413121 0.069826 0.843109 0.028 Uiso 1 1 calc R U . . .
C11 C 0.1592(2) 0.06325(15) 0.45387(14) 0.0201(4) Uani 1 1 d . . . . .
H11A H 0.076029 0.017057 0.428974 0.024 Uiso 1 1 calc R U . . .
H11B H 0.239245 0.039208 0.425097 0.024 Uiso 1 1 calc R U . . .
C12 C 0.12386(19) 0.17762(15) 0.42800(14) 0.0180(4) Uani 1 1 d . . . . .
H12A H 0.101502 0.187056 0.356488 0.022 Uiso 1 1 calc R U . . .
H12B H 0.040838 0.200816 0.454025 0.022 Uiso 1 1 calc R U . . .
C13 C 0.2341(2) 0.34852(16) 0.44249(15) 0.0251(4) Uani 1 1 d . . . . .
H13A H 0.158057 0.381714 0.468888 0.038 Uiso 1 1 calc R U . . .
H13B H 0.210836 0.353135 0.371319 0.038 Uiso 1 1 calc R U . . .
H13C H 0.323774 0.385830 0.467524 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2520(2) -0.04632(15) 0.59041(16) 0.0242(4) Uani 1 1 d . . . . .
H14A H 0.335856 -0.061859 0.563592 0.036 Uiso 1 1 calc R U . . .
H14B H 0.178798 -0.100329 0.567935 0.036 Uiso 1 1 calc R U . . .
H14C H 0.278280 -0.047464 0.661639 0.036 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 Mg1 76.73(6) . . ?
C6 S2 Mg1 76.11(6) . . ?
S1 Mg1 S2 162.48(3) . . ?
O1 Mg1 S1 95.01(4) . . ?
O1 Mg1 S2 98.67(4) . . ?
O1 Mg1 O2 77.65(5) . . ?
O1 Mg1 N1 159.45(6) . . ?
O1 Mg1 N2 94.81(6) . . ?
O2 Mg1 S1 102.07(4) . . ?
O2 Mg1 S2 91.55(4) . . ?
O2 Mg1 N1 95.54(6) . . ?
N1 Mg1 S1 67.17(4) . . ?
N1 Mg1 S2 100.90(5) . . ?
N2 Mg1 S1 101.20(5) . . ?
N2 Mg1 S2 66.88(5) . . ?
N2 Mg1 O2 156.06(6) . . ?
N2 Mg1 N1 98.57(6) . . ?
C11 O1 Mg1 112.90(10) . . ?
C11 O1 C14 111.26(14) . . ?
C14 O1 Mg1 119.61(11) . . ?
C12 O2 Mg1 107.66(10) . . ?
C13 O2 Mg1 120.59(12) . . ?
C13 O2 C12 111.66(14) . . ?
C1 N1 Mg1 100.78(11) . . ?
C5 N1 Mg1 139.85(12) . . ?
C5 N1 C1 119.31(16) . . ?
C6 N2 Mg1 101.16(12) . . ?
C10 N2 Mg1 138.56(14) . . ?
C10 N2 C6 120.04(17) . . ?
N1 C1 S1 115.31(13) . . ?
N1 C1 C2 120.40(17) . . ?
C2 C1 S1 124.29(14) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.51(17) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.84(18) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 121.0 . . ?
C5 C4 C3 117.99(18) . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.92(18) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
N2 C6 S2 115.84(14) . . ?
N2 C6 C7 119.85(18) . . ?
C7 C6 S2 124.30(16) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.02(19) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.8 . . ?
C10 C9 C8 118.4(2) . . ?
C10 C9 H9 120.8 . . ?
N2 C10 C9 122.2(2) . . ?
N2 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
O1 C11 H11A 110.4 . . ?
O1 C11 H11B 110.4 . . ?
O1 C11 C12 106.84(14) . . ?
H11A C11 H11B 108.6 . . ?
C12 C11 H11A 110.4 . . ?
C12 C11 H11B 110.4 . . ?
O2 C12 C11 106.16(15) . . ?
O2 C12 H12A 110.5 . . ?
O2 C12 H12B 110.5 . . ?
C11 C12 H12A 110.5 . . ?
C11 C12 H12B 110.5 . . ?
H12A C12 H12B 108.7 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
O1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 Mg1 2.5595(7) . ?
S1 C1 1.7384(19) . ?
S2 Mg1 2.5818(7) . ?
S2 C6 1.733(2) . ?
Mg1 O1 2.1169(14) . ?
Mg1 O2 2.1355(14) . ?
Mg1 N1 2.1434(16) . ?
Mg1 N2 2.1347(17) . ?
O1 C11 1.436(2) . ?
O1 C14 1.443(2) . ?
O2 C12 1.442(2) . ?
O2 C13 1.435(2) . ?
N1 C1 1.359(2) . ?
N1 C5 1.348(2) . ?
N2 C6 1.357(2) . ?
N2 C10 1.341(3) . ?
C1 C2 1.409(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.411(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.367(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.392(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.380(3) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.500(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 C3 -179.31(15) . . . . ?
S2 C6 C7 C8 -174.45(15) . . . . ?
Mg1 S1 C1 N1 -0.81(12) . . . . ?
Mg1 S1 C1 C2 179.38(17) . . . . ?
Mg1 S2 C6 N2 0.21(12) . . . . ?
Mg1 S2 C6 C7 178.82(17) . . . . ?
Mg1 O1 C11 C12 -34.45(16) . . . . ?
Mg1 O2 C12 C11 -52.24(15) . . . . ?
Mg1 N1 C1 S1 0.96(14) . . . . ?
Mg1 N1 C1 C2 -179.23(14) . . . . ?
Mg1 N1 C5 C4 177.40(15) . . . . ?
Mg1 N2 C6 S2 -0.25(15) . . . . ?
Mg1 N2 C6 C7 -178.93(15) . . . . ?
Mg1 N2 C10 C9 173.17(15) . . . . ?
O1 C11 C12 O2 57.12(18) . . . . ?
N1 C1 C2 C3 0.9(3) . . . . ?
N2 C6 C7 C8 4.1(3) . . . . ?
C1 N1 C5 C4 0.9(3) . . . . ?
C1 C2 C3 C4 0.4(3) . . . . ?
C2 C3 C4 C5 -1.0(3) . . . . ?
C3 C4 C5 N1 0.4(3) . . . . ?
C5 N1 C1 S1 178.70(13) . . . . ?
C5 N1 C1 C2 -1.5(3) . . . . ?
C6 N2 C10 C9 0.2(3) . . . . ?
C6 C7 C8 C9 -1.1(3) . . . . ?
C7 C8 C9 C10 -2.2(3) . . . . ?
C8 C9 C10 N2 2.8(3) . . . . ?
C10 N2 C6 S2 175.02(14) . . . . ?
C10 N2 C6 C7 -3.7(3) . . . . ?
C13 O2 C12 C11 173.25(15) . . . . ?
C14 O1 C11 C12 -172.17(14) . . . . ?
