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_7132934
_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 S2 Tm'
_chemical_formula_sum            'C72 H98 S2 Tm'
_chemical_formula_weight         1196.55
_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             2023-05-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)

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
;
2023-05-07 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                104.3400(10)
_cell_angle_beta                 93.6930(10)
_cell_angle_gamma                98.5700(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2573(10)
_cell_length_b                   14.2636(10)
_cell_length_c                   18.3627(13)
_cell_measurement_reflns_used    9308
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.39
_cell_volume                     3307.9(4)
_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_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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 0.964
_diffrn_measurement_device_type  'Bruker 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  0.0350
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.538
_diffrn_reflns_theta_min         1.151
_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    1.442
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0469 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.8747.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             1262
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane, diethyl ether'
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.112
_refine_diff_density_max         2.452
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         19517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+2.4236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16608
_reflns_number_total             19517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01037j2.cif
_cod_data_source_block           crs268
_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               7132934
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.723
_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. Others
 Fixed Sof: H19(0.45) H19A(0.55) H34(0.6) H34A(0.4) H70(0.5) H70A(0.5)
 C20(0.45) H20A(0.45) H20B(0.45) H20C(0.45) C21(0.45) H21A(0.45) H21B(0.45)
 H21C(0.45) C35(0.6) H35A(0.6) H35B(0.6) H35C(0.6) C36(0.6) H36A(0.6) H36B(0.6)
 H36C(0.6) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) C72(0.5) H72A(0.5) H72B(0.5)
 H72C(0.5) C20A(0.55) H20D(0.55) H20E(0.55) H20F(0.55) C21A(0.55) H21D(0.55)
 H21E(0.55) H21F(0.55) C35A(0.4) H35D(0.4) H35E(0.4) H35F(0.4) C36A(0.4)
 H36D(0.4) H36E(0.4) H36F(0.4) C71A(0.5) H71D(0.5) H71E(0.5) H71F(0.5)
 C72A(0.5) H72D(0.5) H72E(0.5) H72F(0.5)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C19(H19), C19(H19A), C28(H28), C31(H31), C34(H34),
 C34(H34A), C49(H49), C52(H52), C55(H55), C64(H64), C67(H67), C70(H70),
 C70(H70A)
3.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)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), 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), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C20A(H20D,H20E,H20F), C21A(H21D,H21E,
 H21F), C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F), C71A(H71D,H71E,H71F),
 C72A(H72D,H72E,H72F)
;
_shelx_res_checksum              53247
_shelx_hkl_checksum              8400
_olex2_submission_special_instructions 'No special instructions were received'