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_7132936
_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 Nd S2'
_chemical_formula_sum            'C72 H98 Nd S2'
_chemical_formula_weight         1171.86
_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             2023-12-23
_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
;
2024-01-01 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                104.9172(10)
_cell_angle_beta                 93.8221(10)
_cell_angle_gamma                97.9184(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2169(7)
_cell_length_b                   14.2162(8)
_cell_length_c                   18.5245(10)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.29
_cell_volume                     3312.3(3)
_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      93.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_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       0
_diffrn_reflns_number            20371
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.578
_diffrn_reflns_theta_min         1.624
_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    0.885
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0655 before and 0.0561 after correction.
 The Ratio of minimum to maximum transmission is 0.92.

Final HKLF 4 output contains 225868 reflections, Rint = 0.0641
 (72309 with I > 3sig(I), Rint = 0.0487)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.950
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         20371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0543P)^2^+7.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17815
_reflns_number_total             20371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01037j2.cif
_cod_data_source_block           crs285
_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               7132936
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9089(14)
 0.0508(11) 0.0403(9)
2. 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
3. Others
 Fixed Sof: Nd1(0.9) Nd1A(0.1) H34(0.6) H34A(0.4) C35(0.6) H35A(0.6) H35B(0.6)
 H35C(0.6) C35A(0.4) H35D(0.4) H35E(0.4) H35F(0.4) C36(0.6) H36A(0.6) H36B(0.6)
 H36C(0.6) C36A(0.4) H36D(0.4) H36E(0.4) H36F(0.4) 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) H62(0.9)
 H62A(0.1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C19(H19), C28(H28), C31(H31), C34(H34), C34(H34A),
 C49(H49), C49(H49A), C52(H52), C55(H55), C62(H62), C62(H62A), 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), C47(H47), C60(H60)
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),
 C35A(H35D,H35E,H35F), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F), 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)
;
_shelx_res_checksum              57618
_shelx_hkl_checksum              18539
_olex2_submission_special_instructions 'No special instructions were received'