Modulation of the structural information in shape-defined heterocyclic strands: the case of a (pyridine-hydrazone)2pyrazine ligand
Thangavel, Muthu Kumar; Harrowfield, Jack; Bailly, Corinne; Karmazin, Lydia; Stadler, Adrian-Mihail; Dalton Transactions  (2022) –; doi:10.1039/D2DT01684B

data_7711098
_publ_section_title
;
 Modulation of the structural information in shape-defined heterocyclic
 strands: the case of a (pyridine-hydrazone)2pyrazine ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01684B
_journal_year                    2022
_chemical_formula_moiety         'C72 H72 Cd4 N32, 6(C F3 O3 S)'
_chemical_formula_sum            'C78 H72 Cd4 F18 N32 O18 S6'
_chemical_formula_weight         2729.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2681(9)
_cell_length_b                   24.4819(12)
_cell_length_c                   26.1478(12)
_cell_measurement_reflns_used    9293
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.63
_cell_volume                     12334.4(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            129852
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.087
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       prism
_exptl_crystal_F_000             5432
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_platon_squeeze_details
'The residual electron density was assigned to half a molecule of the triflate anion and two molecules of the dimethylsulfoxide solvent [1861/16= 116 e per asymmetric unit; half a molecule of C1F3O3S1 and two molecules of C2H6O1S1 would give 120 e].'
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.347
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         7634
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0938
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+224.9480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2404
_refine_ls_wR_factor_ref         0.2882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4585
_reflns_number_total             7634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01684b1.cif
_cod_data_source_block           Cd4L4
_cod_database_code               7711098
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.669
_shelx_estimated_absorpt_t_max   0.933
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              24094
_shelx_hkl_checksum              5288
_shelx_fab_checksum              50574