Exploring sulfur donor atom coordination chemistry with La(II), Nd(II), and Tm(II) using a terphenylthiolate ligand.
Gilbert-Bass, Kito; Stennett, Cary R.; Grotjahn, Robin; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Chemical communications (Cambridge, England) 60 (2024) 4601–4604; doi:10.1039/d4cc01037j

data_7132938
_publ_section_title
;
 Exploring sulfur donor atom coordination chemistry with La(II), Nd(II),
 and Tm(II) using a terphenylthiolate ligand.
;
_journal_issue                   34
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4601
_journal_page_last               4604
_journal_paper_doi               10.1039/d4cc01037j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C72 H98 I0.129 La S2'
_chemical_formula_sum            'C72 H98 I0.13 La S2'
_chemical_formula_weight         1183.03
_chemical_melting_point          ?
_chemical_properties_physical
Air-sensitive,Moisture-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             2024-02-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-29 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                104.544(2)
_cell_angle_beta                 93.628(2)
_cell_angle_gamma                98.433(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2090(4)
_cell_length_b                   14.2623(4)
_cell_length_c                   18.5499(6)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    92.85
_cell_measurement_theta_max      65.88
_cell_measurement_theta_min      2.47
_cell_volume                     3327.73(18)
_computing_cell_refinement       'Bruker SAINT 8.38a, 2013'
_computing_data_collection       'Bruker APEX3 2017.3-0, 2017'
_computing_data_reduction        'Bruker SAINT 8.38a, 2013'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL 2014/5 (XT)'
_diffrn_ambient_temperature      92.85
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Prospector APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58509
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.448
_diffrn_reflns_theta_min         2.474
_diffrn_source                   'IuS microsource'
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.291
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1243 before and 0.0925 after correction.
The Ratio of minimum to maximum transmission is 0.7209.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1252
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.473
_refine_diff_density_min         -2.264
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         12145
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0874
_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^)+(0.0567P)^2^+25.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8321
_reflns_number_total             12145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01037j2.cif
_cod_data_source_block           kgb46
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7132934--7132940.cif.
;
_cod_database_code               7132938
_shelx_estimated_absorpt_t_max   0.630
_shelx_estimated_absorpt_t_min   0.442
_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. Restrained distances
 C17-C16 \\sim C17A-C16
 with sigma of 0.02
 C50A-C49 \\sim C50-C49 \\sim C51-C49 \\sim C51A-C49
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C74 \\sim C75: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C16 \\sim C17 \\sim C17A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
C50 \\sim C50A \\sim C51 \\sim C51A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C35A(0.5) H35A(0.5) H35B(0.5) H35C(0.5) H16(0.5) H16A(0.5)
 C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C17A(0.5) H17D(0.5) H17E(0.5) H17F(0.5)
 H31(0.6) H31A(0.4) C32(0.6) H32A(0.6) H32B(0.6) H32C(0.6) C33(0.6) H33A(0.6)
 H33B(0.6) H33C(0.6) H34(0.5) H34A(0.5) C35(0.5) H35D(0.5) H35E(0.5) H35F(0.5)
 C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) H49(0.7) H49A(0.3) C50(0.7) H50A(0.7)
 H50B(0.7) H50C(0.7) C50A(0.3) H50D(0.3) H50E(0.3) H50F(0.3) C51(0.7) H51A(0.7)
 H51B(0.7) H51C(0.7) C51A(0.3) H51D(0.3) H51E(0.3) H51F(0.3) C36A(0.5)
 H36D(0.5) H36E(0.5) H36F(0.5) C74(0.4) H74A(0.4) H74B(0.4) H74C(0.4) C75(0.4)
 H75A(0.4) H75B(0.4) H75C(0.4)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C16(H16A), C19(H19), C28(H28), C31(H31), C31(H31A),
 C34(H34), C34(H34A), C49(H49), C49(H49A), C52(H52), C55(H55), C64(H64),
 C67(H67), C70(H70)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C24(H24), C26(H26), C39(H39),
 C40(H40), C41(H41), C45(H45), C47(H47), C60(H60), C62(H62)
5.c Idealised Me refined as rotating group:
 C35A(H35A,H35B,H35C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C35(H35D,H35E,H35F), C36(H36A,H36B,H36C), C50(H50A,
 H50B,H50C), C50A(H50D,H50E,H50F), C51(H51A,H51B,H51C), C51A(H51D,H51E,H51F),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C36A(H36D,H36E,H36F),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              49713
_shelx_hkl_checksum              47752
_olex2_submission_special_instructions 'No special instructions were received'