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_4339771
_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            'C62 H91 Dy3 N26 O27'
_chemical_formula_weight         2120.11
_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                 105.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.980(3)
_cell_length_b                   16.215(4)
_cell_length_c                   21.707(4)
_cell_measurement_reflns_used    23207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.51
_cell_measurement_theta_min      3.07
_cell_volume                     4063.5(17)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30412
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.823
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED; Oxford-Diffraction Poland, 2003'
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2118
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.34
_refine_diff_density_min         -0.49
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         12281
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                10738
_reflns_number_total             12281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700831z-file002.cif
_cod_data_source_block           j3abs
_cod_original_cell_volume        4063.5(16)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4339771