Anion and Solvent Induced Chirality Inversion in Macrocyclic Lanthanide Complexes
Aleksandra Gerus; Katarzyna Ślepokura; Jerzy Lisowski; Inorganic Chemistry 52 (2013) 12450–12460; doi:10.1021/ic401437r

data_4336555
_publ_contact_author_address
;
Department of Chemistry, 
University of Wroclaw, 
14 F. Joliot-Curie
50-383 Wroclaw,
Poland
;
_publ_contact_author_email       jerzy.lisowski@chem.uni.wroc.pl
_publ_contact_author_fax         '+48 71 3282348'
_publ_contact_author_name        'Jerzy Lisowski'
_publ_contact_author_phone       '+48 71 3757252'
_publ_section_title
;
 Anion and Solvent Induced Chirality Inversion in Macrocyclic Lanthanide
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12450
_journal_page_last               12460
_journal_paper_doi               10.1021/ic401437r
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C26 H40 Cl N6 O Yb, 2(Cl), C2 H3 N'
_chemical_formula_sum            'C28 H43 Cl3 N7 O Yb'
_chemical_formula_weight         773.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.969(2)
_cell_length_b                   18.679(5)
_cell_length_c                   20.558(5)
_cell_measurement_reflns_used    21419
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      36.81
_cell_measurement_theta_min      2.77
_cell_volume                     3060.1(13)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type
;
Kuma KM4 CCD kappa-geometry diffractometer with a Sapphire CCD camera
;
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27981
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.095
_diffrn_reflns_theta_min         2.779
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    3.353
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
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            yellowish
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       plate
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 3194 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         8356
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0350P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.810
_reflns_number_gt                7777
_reflns_number_total             8356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401437r_si_002_7.cif
_cod_data_source_block           aku12ab
_cod_database_code               4336555
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.824
_shelxl_version_number           2013-2