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_4108917
_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            'C47 H75 Ce N16 O12'
_chemical_formula_weight         1196.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     vectmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.469(3)
_cell_length_b                   14.537(3)
_cell_length_c                   28.830(6)
_cell_measurement_reflns_used    20210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6741
_cell_measurement_theta_min      2.5994
_cell_volume                     5645(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_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 0.990
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Kuma KM4 with 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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            40745
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
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    1.408
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.2988
_exptl_crystal_size_mid          0.1950
_exptl_crystal_size_min          0.1499
_refine_diff_density_max         1.687
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         13646
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0585P)^2^+5.6613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                11294
_reflns_number_total             13646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805033j_si_002.cif
_cod_data_source_block           cel6abs
_cod_database_code               4108917