A new class of anionic metallohelicates based on salicylic and terephthalic acid units, accessible in solution and by mechanochemistry.
Do, Jean-Louis; Titi, Hatem M.; Cuccia, Louis A.; Friščić, Tomislav; Chemical communications (Cambridge, England) 57 (2021) 5143–5146; doi:10.1039/d0cc08180a

data_7128187
_publ_section_title
;
 A new class of anionic metallohelicates based on salicylic and
 terephthalic acid units, accessible in solution and by mechanochemistry.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5143
_journal_page_last               5146
_journal_paper_doi               10.1039/d0cc08180a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'C54 H65 Cu2 N16 O19'
_chemical_formula_weight         1369.30
_chemical_name_systematic
'(guanidinium)4Cu2(N,N'-bis(3-carboxylate-2-hydroxyphenyl)terephthalamide )2.H2O.iPrOH'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-04-08 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.066(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6408(15)
_cell_length_b                   12.2924(7)
_cell_length_c                   22.7172(12)
_cell_measurement_reflns_used    6380
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.078
_cell_measurement_theta_min      4.428
_cell_volume                     6987.8(7)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_molecular_graphics    'Mercury 4.0 (Wood 2020)'
_computing_publication_material  'enCIFer 2020.2.0'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker AXS D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55069
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.078
_diffrn_reflns_theta_min         4.428
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0406P)^2^+10.9870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6379
_reflns_number_total             6868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08180a2.cif
_cod_data_source_block           CuH2r
_cod_depositor_comments
'Adding full bibliography for 7128186--7128192.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7128187
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.704
_shelx_res_checksum              22271
_shelx_fab_checksum              7061