Helical Lanthanide(III) Complexes with Chiral Nonaaza Macrocycle
Janusz Gregoliński; Przemysław Starynowicz; KimNgan T. Hua; Jamie L. Lunkley; Gilles Muller; Jerzy Lisowski; Journal of the American Chemical Society 130 (2008) 17761–17773; doi:10.1021/ja805033j

data_4108918
_publ_section_title
;
 Helical Lanthanide(III) Complexes with Chiral Nonaaza Macrocycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17761
_journal_page_last               17773
_journal_paper_doi               10.1021/ja805033j
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_sum            'C42.75 H70.13 Lu N13.88 O12.75'
_chemical_formula_weight         1157.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.982(4)
_cell_length_b                   14.982(4)
_cell_length_c                   38.92(2)
_cell_measurement_reflns_used    6793
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      3
_cell_volume                     7566(5)
_computing_cell_refinement       'CrysAlis RED ver. 1.171'
_computing_data_collection       'CrysAlis CCD ver. 1.171'
_computing_data_reduction        'CrysAlis RED ver. 1.171'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Kuma KM4 with a CCD counter'
_diffrn_measurement_method       '\w 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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            50951
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    2.032
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3581
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.818
_refine_diff_density_min         -0.600
_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   -0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         12056
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                8869
_reflns_number_total             12056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805033j_si_003.cif
_cod_data_source_block           grluabs
_cod_original_sg_symbol_H-M      'P 3 2 21'
_cod_database_code               4108918