Ion-pair triple helicates and mesocates self-assembled from ditopic 2,2'-bipyridine-bis(urea) ligands and Ni(II) or Fe(II) sulfate salts
Radu Custelcean; Peter V. Bonnesen; Benjamin D. Roach; Nathan C. Duncan; Chem.Commun. 48 (2012) 7438–; doi:10.1039/c2cc33062h

data_7108024
_publ_section_title
;
 Ion-pair triple helicates and mesocates self-assembled from ditopic
 2,2'-bipyridine-bis(urea) ligands and Ni(II) or Fe(II) sulfate salts
;
_journal_name_full               Chem.Commun.
_journal_page_first              7438
_journal_paper_doi               10.1039/c2cc33062h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C87 H89 N23 Ni O21 S'
_chemical_formula_weight         1883.58
_chemical_name_common            H1b
_chemical_name_systematic
;
?
;
_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           SHELXL-97
_cell_angle_alpha                95.997(2)
_cell_angle_beta                 104.132(2)
_cell_angle_gamma                108.688(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7888(11)
_cell_length_b                   19.1350(15)
_cell_length_c                   19.5872(16)
_cell_measurement_temperature    173(2)
_cell_volume                     4652.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45983
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.9400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         16391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1363P)^2^+0.4837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2147
_reflns_number_gt                11542
_reflns_number_total             16391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33062h.txt
_cod_data_source_block           c:\frames\470\work\470sq
_cod_original_cell_volume        4652.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108024