Series of Lanthanide-Alkali Metal-Organic Frameworks Exhibiting Luminescence and Permanent Microporosity
Chandler, Brett D.; Yu, Joanne O.; Cramb, David T.; Shimizu, George K. H.; Chemistry of Materials 19 (2007) 4467–; doi:10.1021/cm070930i

data_4001382
_publ_section_title
;
 Series of Lanthanide-Alkali Metal-Organic Frameworks Exhibiting
 Luminescence and Permanent Microporosity
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4467
_journal_paper_doi               10.1021/cm070930i
_journal_volume                  19
_journal_year                    2007
_chemical_formula_moiety         'C40 H24 Cl Gd N8 Na6 O40 S8, 0.5(O6), 5(O)'
_chemical_formula_sum            'C40 H24 Cl Gd N8 Na6 O48 S8'
_chemical_formula_weight         1971.87
_chemical_name_common
;catena-(tetrakis(4,4'-Disulfo-2,2'-bipyridine N,N'-dioxide)-
di-aqua-hexa-sodium-gadolinium chloride clathrate hydrate)
;
_chemical_name_systematic
;catena-(tetrakis(4,4'-Disulfo-2,2'-bipyridine N,N'-dioxide)-
di-aqua-hexa-sodium-gadolinium chloride clathrate hydrate)
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      81
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            1
_cell_length_a                   12.234(5)
_cell_length_b                   12.234(5)
_cell_length_c                   12.373(5)
_cell_measurement_reflns_used    7872
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.407
_cell_volume                     1851.9(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1427
_diffrn_reflns_av_sigmaI/netI    0.0948
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15632
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             979
_exptl_crystal_size_max          .329
_exptl_crystal_size_mid          .308
_exptl_crystal_size_min          .227
_refine_diff_density_max         3.174
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.274
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.051(15)
_refine_ls_extinction_coef       0.060(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+3.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                3890
_reflns_number_total             4255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm070930isi20070403_025744.cif
_cod_data_source_block           import
_cod_original_formula_sum        'C40 H24 Cl Gd N8 Na6 O48 S8 '
_cod_database_code               4001382