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_7132937
_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 I La S2'
_chemical_formula_sum            'C72 H98 I La S2'
_chemical_formula_weight         1293.43
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-09-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                102.710(2)
_cell_angle_beta                 94.255(2)
_cell_angle_gamma                99.004(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2786(13)
_cell_length_b                   14.2335(14)
_cell_length_c                   18.6780(19)
_cell_measurement_reflns_used    8749
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.17
_cell_volume                     3379.5(6)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_solution    'Bruker SHELXTL 2014/4 (XT)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.1327
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72180
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.621
_diffrn_reflns_theta_min         1.490
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker, 2014/5) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8648.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         19933
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11152
_reflns_number_total             19933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01037j2.cif
_cod_data_source_block           kgb45
_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               7132937
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.808
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C44 \\sim C44A \\sim C45 \\sim C45A \\sim C46 \\sim C46A \\sim C47 \\sim C47A
\\sim C48 \\sim C48A \\sim C49 \\sim C49A \\sim C50 \\sim C50A \\sim C51 \\sim
C51A \\sim C52 \\sim C52A \\sim C53 \\sim C54 \\sim C54A \\sim C55 \\sim C55A
\\sim C56 \\sim C56A \\sim C57 \\sim C57A: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
3. Others
 Fixed Sof: C44(0.6) C44A(0.4) C45(0.6) H45(0.6) C45A(0.4) H45A(0.4) C46(0.6)
 C46A(0.4) C47(0.6) H47(0.6) C47A(0.4) H47A(0.4) C48(0.6) C48A(0.4) C49(0.6)
 H49(0.6) C49A(0.4) H49A(0.4) C50(0.4) H50A(0.4) H50B(0.4) H50C(0.4) C50A(0.6)
 H50D(0.6) H50E(0.6) H50F(0.6) C51(0.6) H51A(0.6) H51B(0.6) H51C(0.6) C51A(0.4)
 H51D(0.4) H51E(0.4) H51F(0.4) C52(0.6) H52(0.6) C52A(0.4) H52A(0.4) H53A(0.6)
 H53B(0.6) H53C(0.6) H53D(0.4) H53E(0.4) H53F(0.4) C54(0.6) H54A(0.6) H54B(0.6)
 H54C(0.6) C54A(0.4) H54D(0.4) H54E(0.4) H54F(0.4) C55(0.6) H55(0.6) C55A(0.4)
 H55A(0.4) C56(0.6) H56A(0.6) H56B(0.6) H56C(0.6) C56A(0.4) H56D(0.4) H56E(0.4)
 H56F(0.4) C57(0.6) H57A(0.6) H57B(0.6) H57C(0.6) C57A(0.4) H57D(0.4) H57E(0.4)
 H57F(0.4)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C19(H19), C28(H28), C31(H31), C34(H34), C49(H49),
 C49A(H49A), C52(H52), C52A(H52A), C55(H55), C55A(H55A), C64(H64), C67(H67),
 C70(H70)
4.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), C45A(H45A), C47(H47), C47A(H47A), C60(H60),
 C62(H62)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), 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(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C50(H50A,H50B,H50C), C50A(H50D,H50E,H50F), C51(H51A,H51B,
 H51C), C51A(H51D,H51E,H51F), C53(H53A,H53B,H53C), C53(H53D,H53E,H53F),
 C54(H54A,H54B,H54C), C54A(H54D,H54E,H54F), C56(H56A,H56B,H56C), C56A(H56D,H56E,
 H56F), C57(H57A,H57B,H57C), C57A(H57D,H57E,H57F), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              57459
_shelx_hkl_checksum              42561
_olex2_submission_special_instructions 'No special instructions were received'