Enantiopure, Supramolecular Helices Containing Three-Dimensional Tetranuclear Lanthanide(III) Arrays: Synthesis, Structure, Properties, and Solvent-Driven Trinuclear/Tetranuclear Interconversion
Marco Lama; Olimpia Mamula; Gregg S. Kottas; Luisa De Cola; Helen Stoeckli-Evans; Sergiu Shova; Inorganic Chemistry 47 (2008) 8000–8015; doi:10.1021/ic7021006

data_4305166
_publ_section_title
;
Enantiopure, Supramolecular Helices Containing Three-Dimensional
Tetranuclear Lanthanide(III) Arrays: Synthesis, Structure, Properties, and
Solvent-Driven Trinuclear/Tetranuclear Interconversion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8000
_journal_page_last               8015
_journal_paper_doi               10.1021/ic7021006
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C162 H154 N18 Nd4 O19, 2(Cl O4), 9.5(C2 H3 N)'
_chemical_formula_sum            'C181 H182.5 Cl2 N27.5 Nd4 O27'
_chemical_formula_weight         3822.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.837(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.647(2)
_cell_length_b                   27.723(3)
_cell_length_c                   18.681(2)
_cell_measurement_reflns_used    441
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.412
_cell_measurement_theta_min      3.448
_cell_volume                     8620.5(17)
_computing_cell_refinement       'DIRAX (Bruker AXS BV)'
_computing_data_collection       'COLLECT (Bruker AXS BV)'
_computing_data_reduction        'EVALCCD (Bruker AXS BV)'
_computing_molecular_graphics    'PLATON  (Spek, 2003)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker nonius Kappa Apex II CCD'
_diffrn_measurement_method       'Phi & omega scans'
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.868837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3902
_exptl_crystal_size_max          1.02
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.69
_refine_diff_density_max         1.676
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1918
_refine_ls_number_reflns         32300
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+1.7122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                30749
_reflns_number_total             32300
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic7021006-file001.cif
_cod_data_source_block           ml14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C181 H182.50 Cl2 N27.50 Nd4 O27'
_cod_database_code               4305166