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_7063204
_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         'C128 H78 Cu6 N30 O16, 1.5[CH3OH]'
_chemical_formula_sum            'C129.5 H84 Cu6 N30 O17.5'
_chemical_formula_weight         2721.50
_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
_atom_sites_solution_primary     dual
_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                76.085(2)
_cell_angle_beta                 70.053(2)
_cell_angle_gamma                81.249(2)
_cell_formula_units_Z            1
_cell_length_a                   12.8621(7)
_cell_length_b                   14.6778(8)
_cell_length_c                   17.1404(9)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      2.30
_cell_volume                     2943.8(3)
_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 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  0.1174
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            343382
_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         25.996
_diffrn_reflns_theta_min         2.115
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0930 before and 0.0846 after correction.
The Ratio of minimum to maximum transmission is 0.8938.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             1385
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         11552
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+4.8870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9405
_reflns_number_total             11552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01330a2.cif
_cod_data_source_block           Complex1_21mb_orde1_mbrack1_cul10_0m
_cod_depositor_comments
'Adding full bibliography for 7063204--7063206.cif.'
_cod_original_formula_sum        'C129.50 H84 Cu6 N30 O17.50'
_cod_database_code               7063204
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.884
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O8-H8
 0.87 with sigma of 0.01
 Cu2-H8
 2.782412 with sigma of 0.02
 C64-H8
 1.885316 with sigma of 0.02
 Cu1-H7A \\sim Cu1-H7B
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13), C16(H16),
 C17(H17), C18(H18), C20(H20), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31),
  C32(H32), C34(H34), C37(H37), C38(H38), C39(H39), C41(H41), C45(H45),
 C46(H46), C47(H47), C51(H51), C52(H52), C53(H53), C55(H55), C58(H58), C59(H59),
  C60(H60), C62(H62)
3.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C)
;
_shelx_res_checksum              6623
_shelx_fab_checksum              14665
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'