Incorporation of Trinuclear Lanthanide(III) Hydroxo Bridged Clusters in Macrocyclic Frameworks
Michał J. Kobyłka; Katarzyna Ślepokura; Maria Acebrón Rodicio; Marta Paluch; Jerzy Lisowski; Inorganic Chemistry 52 (2013) 12893–12903; doi:10.1021/ic400508y

data_4336690
_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
;
 Incorporation of Trinuclear Lanthanide(III) Hydroxo Bridged Clusters in
 Macrocyclic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12893
_journal_page_last               12903
_journal_paper_doi               10.1021/ic400508y
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C116 H206 Gd6 N20 O46'
_chemical_formula_weight         3560.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 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                 109.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.783(4)
_cell_length_b                   20.900(4)
_cell_length_c                   21.933(4)
_cell_measurement_reflns_used    18840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.78
_cell_measurement_theta_min      2.85
_cell_volume                     7257(3)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type
;
Kuma KM4 CCD kappa-geometry diffractometer with a Sapphire CCD camera
;
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31314
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.650
_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    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(9)
_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     847
_refine_ls_number_reflns         17583
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                15002
_reflns_number_total             17583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400508y_si_002_6.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4336690