Selective anion encapsulation in solid-state Ln(iii)[15-metallacrown-5](3+) compartments through secondary sphere interactions.
Jankolovits, Joseph; Cutland Van-Noord, Annabel D; Kampf, Jeff W.; Pecoraro, Vincent L.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 9803–9808; doi:10.1039/c3dt50535a

data_7021460
_publ_section_title
;
 Selective anion encapsulation in solid-state
 Ln(iii)[15-metallacrown-5](3+) compartments through secondary sphere
 interactions.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9803
_journal_page_last               9808
_journal_paper_doi               10.1039/c3dt50535a
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
(GdCu5C50H60N10O10)2(C6H8O4)2(NO3)2(H2O)17.25
;
_chemical_formula_sum            'C112 H170.5 Cu10 Gd2 N22 O51.25'
_chemical_formula_weight         3595.10
_chemical_name_systematic
;
Gd[15-MC Cu(II), L-homophenylalanineHA-5](adipate)(nitrate)0.5
;
_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                 96.3360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.0407(8)
_cell_length_b                   29.2565(15)
_cell_length_c                   15.7377(8)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.26
_cell_volume                     6882.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'phi and 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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            235088
_diffrn_reflns_theta_full        29.64
_diffrn_reflns_theta_max         29.64
_diffrn_reflns_theta_min         1.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.554
_exptl_absorpt_correction_T_max  0.6564
_exptl_absorpt_correction_T_min  0.4436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, R. Acta Cryst. (1995) A51 33-38.
Sheldrick, G. SADABS (Version 2008/1) Bruker AXS area
detector absorption and other corrections, University of
Gottingen, Germany 2008.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3649
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1938
_refine_ls_number_reflns         38740
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+4.1791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                37660
_reflns_number_total             38740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50535a.txt
_cod_data_source_block           jj115g
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_original_formula_sum        'C112 H170.50 Cu10 Gd2 N22 O51.25'
_cod_database_code               7021460