Facile interconversion of mesitylcopper into a CuMes-Cu<sub>2</sub>bis(amidinate) triangle and a tetracuprous Möbius strip.
Dowling, Keri; Kruczyński, Tomasz; Dutta, Sanjay; Le, D. P. Ngan; Gozem, Samer; McMillen, Colin D.; Bhuvanesh, Nattamai; Stollenz, Michael; Chemical communications (Cambridge, England) 60 (2024) 11136–11139; doi:10.1039/d4cc03935a

data_7133729
_publ_section_title
;
 Facile interconversion of mesitylcopper into a
 CuMes-Cu<sub>2</sub>bis(amidinate) triangle and a tetracuprous
 M&#xf6;bius strip.
;
_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11136
_journal_page_last               11139
_journal_paper_doi               10.1039/d4cc03935a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C34 H47 Cu3 N6'
_chemical_formula_sum            'C34 H47 Cu3 N6'
_chemical_formula_weight         730.39
_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     dual
_audit_creation_date             2023-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                88.712(4)
_cell_angle_beta                 86.426(4)
_cell_angle_gamma                71.457(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6701(10)
_cell_length_b                   12.8540(15)
_cell_length_c                   15.977(2)
_cell_measurement_reflns_used    5033
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      25.740
_cell_measurement_theta_min      2.554
_cell_volume                     1684.8(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX 4 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19251
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.853
_diffrn_reflns_theta_min         2.482
_diffrn_source                   'Bruker QUEST Mo-IuS'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1199 before and 0.0545 after correction.
 
For component 2:
 wR2(int) was 0.0941 before and 0.0584 after correction.
 The Ratio of minimum to maximum transmission is 0.87.

Final HKLF 4 output contains 46087 reflections, Rint = 0.0786
 (29613 with I > 3sig(I), Rint = 0.0669)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       column
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.040
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         19251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+8.2249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15469
_reflns_number_total             19251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03935a3.cif
_cod_data_source_block           ms_tkg33
_cod_depositor_comments
'Adding full bibliography for 7133729--7133731.cif.'
_cod_original_cell_volume        1684.8(3)
_cod_database_code               7133729
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.619
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.575(2)
 0.425(2)
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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C21(H21), C22(H22), C23(H23), C28(H28), C30(H30)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C25(H25A,H25B,
 H25C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              26008
_shelx_hkl_checksum              66410
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id MSB_230703_Q_TKG33
_olex2_submission_special_instructions 'No special instructions were received'