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_7132940
_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         'C84 H108 N2 Nd S2'
_chemical_formula_sum            'C84 H108 N2 Nd S2'
_chemical_formula_weight         1354.08
_chemical_melting_point          ?
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-19 deposited with the CCDC.	2024-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9566(15)
_cell_length_b                   18.7918(17)
_cell_length_c                   24.254(2)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.32
_cell_volume                     7272.6(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0636
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            96047
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.651
_diffrn_reflns_theta_min         2.109
_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    0.816
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0700 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.9203.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.152
_refine_diff_density_max         1.465
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         11139
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0545P)^2^+4.5279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8027
_reflns_number_total             11139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01037j2.cif
_cod_data_source_block           crs288
_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               7132940
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.789
_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. Uiso/Uaniso restraints and constraints
C32 \\sim C32A \\sim C33 \\sim C33A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
3. Others
 Fixed Sof: H34(0.5) H34A(0.5) H31(0.7) H31A(0.3) C35(0.5) H35A(0.5) H35B(0.5)
 H35C(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C32(0.7) H32A(0.7) H32B(0.7)
 H32C(0.7) C33(0.7) H33A(0.7) H33B(0.7) H33C(0.7) C33A(0.3) H33D(0.3) H33E(0.3)
 H33F(0.3) C32A(0.3) H32D(0.3) H32E(0.3) H32F(0.3) C36A(0.5) H36D(0.5)
 H36E(0.5) H36F(0.5) C35A(0.5) H35D(0.5) H35E(0.5) H35F(0.5)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C28(H28), C34(H34), C34(H34A), C16(H16), C19(H19), C31(H31),
 C31(H31A)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C3(H3), C4(H4), C5(H5), C9(H9), C26(H26), C38(H38), C11(H11),
 C42(H42), C39(H39), C40(H40), C41(H41)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C20(H20A,H20B,
 H20C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F), C32A(H32D,H32E,H32F), C36A(H36D,
 H36E,H36F), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              93100
_shelx_hkl_checksum              46183
_olex2_submission_special_instructions 'No special instructions were received'