Supramolecular chemistry of two new bis(1,2,3-triazolyl)pyridine macrocycles: metal complexation, self-assembly and anion binding.
David, Arthur H. G.; Goodwin, Rosemary J.; White, Nicholas G.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1902–1912; doi:10.1039/d2dt03985k

data_7712190
_publ_section_title
;
 Supramolecular chemistry of two new bis(1,2,3-triazolyl)pyridine
 macrocycles: metal complexation, self-assembly and anion binding.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1902
_journal_page_last               1912
_journal_paper_doi               10.1039/d2dt03985k
_journal_volume                  52
_journal_year                    2023
_chemical_compound_source        synthesized
_chemical_formula_moiety
'2(C37 H35 N9 O6), 2(C16 H36 N), C2 H3 N, 0.5(H 2 O), 2(Br)'
_chemical_formula_sum            'C108 H146 Br2 N21 O12.5'
_chemical_formula_weight         2098.29
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2022-12-12 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                106.89(3)
_cell_angle_beta                 90.64(3)
_cell_angle_gamma                92.77(3)
_cell_formula_units_Z            2
_cell_length_a                   16.286(3)
_cell_length_b                   16.323(3)
_cell_length_c                   21.177(4)
_cell_measurement_reflns_used    37252
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.01
_cell_volume                     5378.6(19)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_unetI/netI     0.067
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37252
_diffrn_reflns_theta_full        25.053
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.824
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2222
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.59
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         20281
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.0253981
_refine_ls_shift/su_mean         0.0000756
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ + 2.29P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1774
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1774
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              19
_reflns_limit_k_min              -20
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                17253
_reflns_number_total             20284
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      52.16
_oxford_refine_ls_scale          0.14276(6)
_cod_data_source_file            d2dt03985k4.cif
_cod_data_source_block           8Br
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7712183--7712190.cif.
;
_cod_original_cell_volume        5378(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C108 H146 Br2 N21 O12.50'
_cod_database_code               7712190
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0686
_reflns_number_all               20281