Structural basis for Cu(ii) metallocycle hexamer formation
Bracken, Matthew L.; Fernandes, Manuel A.; Wamwangi, Daniel; Munro, Orde Q.; New Journal of Chemistry 48 (2024) 8994–8999; doi:10.1039/D4NJ01330A

data_7063205
_publ_section_title
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 Structural basis for Cu(ii) metallocycle hexamer formation
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_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8994
_journal_page_last               8999
_journal_paper_doi               10.1039/D4NJ01330A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C114 H86 Cu6 N18 O16, C2 H6 O2, 5(C H4 O)'
_chemical_formula_sum            'C121 H112 Cu6 N18 O23'
_chemical_formula_weight         2567.52
_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   mixed
_audit_creation_date             2024-04-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2024-04-30 deposited with the CCDC.	2024-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                106.572(5)
_cell_angle_beta                 100.636(5)
_cell_angle_gamma                107.752(5)
_cell_formula_units_Z            1
_cell_length_a                   10.8162(11)
_cell_length_b                   17.0096(16)
_cell_length_c                   17.4195(16)
_cell_measurement_reflns_used    2396
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      20.17
_cell_measurement_theta_min      2.44
_cell_volume                     2793.0(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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.3031
_diffrn_reflns_av_unetI/netI     0.1282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            94743
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         1.277
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0991 after correction.
The Ratio of minimum to maximum transmission is 0.7929.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             1322
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         7314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0450P)^2^+15.0840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4071
_reflns_number_total             7314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01330a2.cif
_cod_data_source_block           Complex3_23mbb_bracken_cu12
_cod_depositor_comments
'Adding full bibliography for 7063204--7063206.cif.'
_cod_database_code               7063205
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_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 O(H) groups, All O(H,H) groups
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C47(H47),
  C48(H48), C49(H49), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57)
2.d Tetrahedral OH refined with riding coordinates:
 O9(H9A)
;
_shelx_res_checksum              10978
_shelx_fab_checksum              68553
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'