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_7132935
_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 Nd S2'
_chemical_formula_sum            'C72 H98 I Nd S2'
_chemical_formula_weight         1298.76
_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             2023-12-03
_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
;
2023-12-03 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                102.4330(10)
_cell_angle_beta                 94.7210(10)
_cell_angle_gamma                99.2870(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3492(8)
_cell_length_b                   14.1047(8)
_cell_length_c                   18.6556(11)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    133.15
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.36
_cell_volume                     3360.2(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      133.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.960
_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            68604
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.534
_diffrn_reflns_theta_min         1.504
_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    1.332
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0493 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.9396.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1350
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.142
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         19753
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0345P)^2^+2.2273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15869
_reflns_number_total             19753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01037j2.cif
_cod_data_source_block           crs281
_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               7132935
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.729
_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
 C70A-C63A = C70-C63
 1.54 with sigma of 0.01
 C71A-C70A = C71-C70
 1.54 with sigma of 0.01
 C53A-C52 = C53-C52
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C59 \\sim C59A \\sim C60 \\sim C60A \\sim C61 \\sim C61A \\sim C62 \\sim C62A
\\sim C63 \\sim C63A \\sim C64 \\sim C64A \\sim C65 \\sim C65A \\sim C66 \\sim
C66A \\sim C67 \\sim C67A \\sim C68 \\sim C68A \\sim C69 \\sim C69A \\sim C70
\\sim C70A \\sim C71 \\sim C71A \\sim C72 \\sim C72A: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C16 \\sim C17 \\sim C17A \\sim C18 \\sim C18A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C52 \\sim C53 \\sim C53A \\sim C54: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
4. Others
 Sof(H52A)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(1)
 Sof(H52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(1)
 Fixed Sof: H16(0.6) H16A(0.4) C17(0.6) H17A(0.6) H17B(0.6) H17C(0.6)
 C17A(0.4) H17D(0.4) H17E(0.4) H17F(0.4) C18(0.6) H18A(0.6) H18B(0.6) H18C(0.6)
 C18A(0.4) H18D(0.4) H18E(0.4) H18F(0.4) C59(0.75) C59A(0.25) C60(0.75)
 H60(0.75) C60A(0.25) H60A(0.25) C61(0.75) C61A(0.25) C62(0.75) H62(0.75)
 C62A(0.25) H62A(0.25) C63(0.75) C63A(0.25) C64(0.75) H64(0.75) C64A(0.25)
 H64A(0.25) C65(0.75) H65A(0.75) H65B(0.75) H65C(0.75) C65A(0.25) H65D(0.25)
 H65E(0.25) H65F(0.25) C66(0.75) H66A(0.75) H66B(0.75) H66C(0.75) C66A(0.25)
 H66D(0.25) H66E(0.25) H66F(0.25) C67(0.75) H67(0.75) C67A(0.25) H67A(0.25)
 C68(0.75) H68A(0.75) H68B(0.75) H68C(0.75) C68A(0.25) H68D(0.25) H68E(0.25)
 H68F(0.25) C69(0.75) H69A(0.75) H69B(0.75) H69C(0.75) C69A(0.25) H69D(0.25)
 H69E(0.25) H69F(0.25) C70(0.75) H70(0.75) C70A(0.25) H70A(0.25) C71(0.75)
 H71A(0.75) H71B(0.75) H71C(0.75) C71A(0.25) H71D(0.25) H71E(0.25) H71F(0.25)
 C72(0.75) H72A(0.75) H72B(0.75) H72C(0.75) C72A(0.25) H72D(0.25) H72E(0.25)
 H72F(0.25)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C16(H16A), C19(H19), C28(H28), C31(H31), C34(H34),
 C49(H49), C52(H52), C52(H52A), C55(H55), C64(H64), C64A(H64A), C67(H67),
 C67A(H67A), C70(H70), C70A(H70A)
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), C60A(H60A), C62(H62),
 C62A(H62A)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C17A(H17D,H17E,
 H17F), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), 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), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C53A(H53D,H53E,H53F),
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C65(H65A,H65B,
 H65C), C65A(H65D,H65E,H65F), C66(H66A,H66B,H66C), C66A(H66D,H66E,H66F),
 C68(H68A,H68B,H68C), C68A(H68D,H68E,H68F), C69(H69A,H69B,H69C), C69A(H69D,H69E,
 H69F), C71(H71A,H71B,H71C), C71A(H71D,H71E,H71F), C72(H72A,H72B,H72C),
 C72A(H72D,H72E,H72F)
;
_shelx_res_checksum              16317
_shelx_hkl_checksum              17699
_olex2_submission_special_instructions 'No special instructions were received'