Probing the nature of intramolecular (sp<sup>3</sup>)C-H⋯Cu(I) interactions in organo thione copper(I) cages.
Ramakant, Girbide Amitkumar; Muduli, Gopendra; Rai, Rakesh Kumar; Prabusankar, Ganesan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3118–3126; doi:10.1039/d4dt03294b

data_7717822
_publ_section_title
;
 Probing the nature of intramolecular (sp<sup>3</sup>)C-H&#x22ef;Cu(I)
 interactions in organo thione copper(I) cages.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3118
_journal_page_last               3126
_journal_paper_doi               10.1039/d4dt03294b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C74 H68 Cu4 I4 N12 S4, [+ solvents]'
_chemical_formula_sum            'C74 H68 Cu4 I4 N12 S4'
_chemical_formula_weight         2015.510
_chemical_name_systematic        SCuI
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-10 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                72.964(4)
_cell_angle_beta                 78.573(5)
_cell_angle_gamma                89.436(4)
_cell_formula_units_Z            1
_cell_length_a                   10.2882(14)
_cell_length_b                   14.6183(17)
_cell_length_c                   15.560(2)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      25.994
_cell_measurement_theta_min      2.432
_cell_volume                     2190.2(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9987
_diffrn_measurement_device_type  'Bruker APEX-V Photon II'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60706
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9987
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         2.02
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.506
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0734 after correction.
The Ratio of minimum to maximum transmission is 0.7606.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             988.791
_exptl_crystal_preparation       'SLOW EVAPORATION'
_exptl_crystal_recrystallization_method
'The material was recrystallised from CH3CN by slow evaporation'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.7039
_refine_diff_density_min         -1.1723
_refine_diff_density_rms         0.1464
_refine_ls_d_res_high            0.7786
_refine_ls_d_res_low             10.0709
_refine_ls_goodness_of_fit_ref   1.0194
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     730
_refine_ls_number_reflns         9699
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.0145
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.9241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6921
_reflns_number_total             9699
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03294b2.cif
_cod_data_source_block           mo_2_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7717819--7717822.cif.'
_cod_original_cell_volume        2190.3(5)
_cod_database_code               7717822
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(Cu1)
Uanis(S2) = Uanis(Cu2)
Uanis(H14a) = Uanis(H14b)
2. Rigid body (RIGU) restrains
 C7, H7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, H25c
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, H30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, H6b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, H37b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, H25b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H14b, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H26c, H26b, C26, H26a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H18a, C18, H18b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H13, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, H6b, H6a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, H4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, H37a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H14a, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, H14a, H14b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H14b, C14, H14a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H34, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H23a, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, H14a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         PBE
   BASIS SET:      ECP-def2-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2025-01-07_14-48-20
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'nylone loop'
_olex2_submission_special_instructions 'No special instructions were received'