Lanthanide complexes of the chiral hexaaza macrocycle and its meso-type isomer: solvent-controlled helicity inversion.
Gregoliński, Janusz; Slepokura, Katarzyna; Lisowski, Jerzy; Inorganic chemistry 46 (2007) 7923–7934; doi:10.1021/ic700831z

data_4339770
_publ_section_title
;
 Lanthanide complexes of the chiral hexaaza macrocycle and its meso-type
 isomer: solvent-controlled helicity inversion.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7923
_journal_page_last               7934
_journal_paper_doi               10.1021/ic700831z
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C26 H42 Eu N9 O11'
_chemical_formula_weight         808.65
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 105.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.292(3)
_cell_length_b                   15.103(3)
_cell_length_c                   15.524(3)
_cell_measurement_reflns_used    30386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.48
_cell_measurement_theta_min      3.03
_cell_volume                     3228.7(12)
_computing_cell_refinement       'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_data_collection       'CrysAlis CCD; Oxford-Diffraction Poland, 2003'
_computing_data_reduction        'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
KUMA KM4 kappa-geometry diffractometer with Saphire CCD camera
;
_diffrn_measurement_method       'omega scan'
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29828
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.80
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         12240
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                11559
_reflns_number_total             12240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700831z-file002.cif
_cod_data_source_block           gr1sabs
_cod_original_cell_volume        3228.7(11)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4339770