CP/MAS NMR studies on binding environment of CH3CN in Cu(i) complexes with disilane-bridged bis(methylpyridine) ligands
Sato, Kei-ichi; Hattori, Mineyuki; Yamanoi, Yoshinori; RSC Advances 15 (2025) 16968–16972; doi:10.1039/D5RA02962G

data_7250423
_publ_section_title
;
 CP/MAS NMR studies on binding environment of CH3CN in Cu(i) complexes
 with disilane-bridged bis(methylpyridine) ligands
;
_journal_issue                   21
_journal_name_full               'RSC Advances'
_journal_page_first              16968
_journal_page_last               16972
_journal_paper_doi               10.1039/D5RA02962G
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C36 H54 Cu4 I4 N6 Si4'
_chemical_formula_sum            'C36 H54 Cu4 I4 N6 Si4'
_chemical_formula_weight         1444.97
_chemical_name_systematic        20221107L1CuI100K
_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     iterative
_audit_creation_date             2025-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-04-25 deposited with the CCDC.	2025-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                81.667(2)
_cell_angle_beta                 74.5990(10)
_cell_angle_gamma                64.2270(10)
_cell_formula_units_Z            1
_cell_length_a                   9.3981(5)
_cell_length_b                   10.1021(6)
_cell_length_c                   14.9219(8)
_cell_measurement_reflns_used    3833
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.55
_cell_volume                     1229.25(12)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      112.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21518
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.338
_diffrn_reflns_theta_min         2.240
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6820
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0704 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.9152.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0198P)^2^+2.1346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3532
_reflns_number_total             4493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra02962g2.cif
_cod_data_source_block           mo_20221107l1cui100k_0m_a
_cod_database_code               7250423
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.646
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              67353
_shelx_hkl_checksum              46147
_olex2_submission_special_instructions 'No special instructions were received'