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_7063206
_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         'C130 H76 Cu6 N32 O14, 4(C2 H3 N)'
_chemical_formula_sum            'C138 H88 Cu6 N36 O14'
_chemical_formula_weight         2855.68
_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                106.667(3)
_cell_angle_beta                 95.920(3)
_cell_angle_gamma                110.424(3)
_cell_formula_units_Z            1
_cell_length_a                   14.4764(11)
_cell_length_b                   15.1477(11)
_cell_length_c                   16.4380(10)
_cell_measurement_reflns_used    9356
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.35
_cell_volume                     3152.1(4)
_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)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.1107
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            162903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.430
_diffrn_reflns_theta_min         2.031
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6027
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1432 before and 0.0849 after correction.
The Ratio of minimum to maximum transmission is 0.8082.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       needle
_exptl_crystal_F_000             1454
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         15772
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0604P)^2^+4.0233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12159
_reflns_number_total             15772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01330a2.cif
_cod_data_source_block           Complex2_23mbb_bracken_cu
_cod_depositor_comments
'Adding full bibliography for 7063204--7063206.cif.'
_cod_database_code               7063206
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.768
_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,H) groups
2. Restrained distances
 Cu2-H7A \\sim Cu2-H7B
 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C31(H31),
  C32(H32), C33(H33), C37(H37), C38(H38), C40(H40), C41(H41), C44(H44),
 C45(H45), C47(H47), C48(H48), C52(H52), C53(H53), C54(H54), C58(H58), C59(H59),
  C61(H61), C62(H62)
3.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C)
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_shelx_res_checksum              50329
_olex2_submission_special_instructions 'No special instructions were received'