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_4336552
_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 H42 N6 O2 Tm, 3(N O3), H2 O'
_chemical_formula_sum            'C26 H44 N9 O12 Tm'
_chemical_formula_weight         843.63
_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     isomor
_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                   10.692(3)
_cell_length_b                   12.469(3)
_cell_length_c                   24.045(6)
_cell_measurement_reflns_used    28297
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.50
_cell_measurement_theta_min      4.70
_cell_volume                     3205.6(14)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Xcalibur PX kappa-geometry diffractometer with an Onyx CCD camera
;
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32691
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         4.710
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    2.844
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.576
_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            colorless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 3240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.027(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7702
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0220P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0360
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7462
_reflns_number_total             7702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401437r_si_002_4.cif
_cod_data_source_block           aku4abs
_cod_database_code               4336552
_shelx_estimated_absorpt_t_min   0.445
_shelx_estimated_absorpt_t_max   0.871
_shelxl_version_number           2013-2