Lanthanide Complexes of the Heterochiral Nonaaza Macrocycle: Switching the Orientation of the Helix Axis
Janusz Gregoliński; Tadeusz Lis; Marta Cyganik; Jerzy Lisowski; Inorganic Chemistry 47 (2008) 11527–11534; doi:10.1021/ic8005986

data_4305621
_publ_contact_author_address
;
Department of Chemistry,
University of Wroclaw,
14 F. Joliot-Curie
50-383 Wroclaw,
Poland
;
_publ_contact_author_email       jurekl@wchuwr.pl
_publ_contact_author_fax         '+48 71 3282348'
_publ_contact_author_name        'Jerzy Lisowski'
_publ_contact_author_phone       '48 71 3757 252'
_publ_section_title
;
Lanthanide Complexes of the Heterochiral Nonaaza Macrocycle: Switching the
Orientation of the Helix Axis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11527
_journal_page_last               11534
_journal_paper_doi               10.1021/ic8005986
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C39 H57 N9 Pr, N6 O18 Pr, C H4 O'
_chemical_formula_sum            'C40 H61 N15 O19 Pr2'
_chemical_formula_weight         1337.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.135(5)
_cell_length_b                   19.326(8)
_cell_length_c                   23.497(10)
_cell_measurement_reflns_used    14339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.94
_cell_measurement_theta_min      2.96
_cell_volume                     5047(4)
_computing_cell_refinement       'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_computing_data_collection       'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_computing_data_reduction        'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_computing_molecular_graphics    'ORTEP III (Farrugia, 1997 )'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type
'Xcalibur PX \k-geometry diffractometer CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.1226
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39071
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         76.94
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    15.408
_exptl_absorpt_correction_T_max  0.5777
_exptl_absorpt_correction_T_min  0.3720
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis Red (Oxford Diffraction, 1995-2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       multifaced
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         9165
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                5129
_reflns_number_total             9165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8005986_si_003_3.cif
_cod_data_source_block           gr81abs
_cod_database_code               4305621