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_7712187
_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         'C37 H35 Br N9 O6 Pd, B F4, C4 H10 O'
_chemical_formula_sum            'C41 H45 B Br F4 N9 O7 Pd'
_chemical_formula_weight         1048.97
_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
;
2022-12-08 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                66.81(3)
_cell_angle_beta                 81.10(3)
_cell_angle_gamma                71.56(3)
_cell_formula_units_Z            2
_cell_length_a                   13.238(3)
_cell_length_b                   13.973(3)
_cell_length_c                   14.000(3)
_cell_measurement_reflns_used    28059
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.58
_cell_volume                     2256.8(11)
_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 0.867
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device       'ADSC Quantum 210r'
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_unetI/netI     0.043
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28059
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         1.583
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.372
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.36
_refine_diff_density_min         -2.19
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         7831
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.0007054
_refine_ls_shift/su_mean         0.0000236
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ + 1.05P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1527
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1527
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6909
_reflns_number_total             7831
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.47
_oxford_diffrn_Wilson_scale      26.24
_oxford_refine_ls_scale          0.17456(13)
_cod_data_source_file            d2dt03985k4.cif
_cod_data_source_block           PdBr_8_acetonitrile
_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        2256.8(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7712187
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0557
_reflns_number_all               7831