Conformational polymorphism in a Schiff-base macrocyclic organic ligand: an experimental and theoretical study
Lo Presti, Leonardo; Soave, Raffaella; Longhi, Mariangela; Ortoleva, Emanuele; Acta Crystallographica Section B 66 (2010) 527–543; doi:10.1107/S0108768110029514

data_2017781
_publ_section_title
;
 Conformational polymorphism in a Schiff-base macrocyclic organic ligand:
 an experimental and theoretical study
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              527
_journal_page_last               543
_journal_paper_doi               10.1107/S0108768110029514
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         '3(C24 H30 N6),2(C2 H3 N),0.68(O)'
_chemical_formula_sum            'C76 H96 N20 O0.68'
_chemical_formula_weight         1300.67
_chemical_melting_point          417.15
_chemical_name_systematic
;
'3,6,9,17,20,23-hexa-azapentacyclo(23.3.1.1^11,15^.0^2,6^.0^16,20^)triaconta
-1(29),9,11,13,15(30),23,25,27-octaene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.378(3)
_cell_angle_beta                 68.153(3)
_cell_angle_gamma                79.441(3)
_cell_formula_units_Z            1
_cell_length_a                   12.2369(14)
_cell_length_b                   12.5634(13)
_cell_length_c                   13.0094(14)
_cell_measurement_reflns_used    1136
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.510
_cell_measurement_theta_min      2.228
_cell_volume                     1824.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS Smart'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_sigmaI/netI    0.1644
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22307
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8495
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2007/4
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             697.6
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.137
_refine_ls_extinction_coef       0.0033(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.2135
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                2729
_reflns_number_total             8389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ps5007.cif
_cod_data_source_block           dienSOLV
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017781