Lanthanide Metal−Organic Frameworks Based on Octahedral Secondary Building Units: Rare Net Topology and Luminescence
Yan, Li; Yue, Qi; Jia, Qin-Xiang; Lemercier, Gilles; Gao, En-Qing; Crystal Growth & Design 9 (2009) 2984–; doi:10.1021/cg9000736

data_4509449
_publ_section_title
;
 Lanthanide Metal&#x2212;Organic Frameworks Based on Octahedral Secondary
 Building Units: Rare Net Topology and Luminescence
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2984
_journal_paper_doi               10.1021/cg9000736
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C63 H71 Eu2 N7 O27 S3'
_chemical_formula_weight         1758.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.8010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.8041(14)
_cell_length_b                   14.8602(6)
_cell_length_c                   29.7740(12)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.24
_cell_volume                     15217.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            92831
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  0.8133
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             7104
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The structure has a large volume fraction of solvent-accessible voids (31%
 of the unit cell volume) containing a number of residual electron density
 peaks attributable to lattice solvent molecules (water and DMF), which 
 were heavily disordered and could not be satisfactorily refined to
 a reasonable disorder model even using the data collected at low temperature
 (123 K). Given that the refinement of the metal-organic coordination
 framework is essentially uninfluenced by the presence of the disordered
 solvent, the SQUEEZE routine in the PLATON software package [A.L. Spek,
 J. Appl. Crystallogr. 2003, 36, 7-13.] was applied to subtract the
 diffraction contribution from the solvent molecules.
;
_refine_diff_density_max         2.565
_refine_diff_density_min         -2.213
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         14937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                11242
_reflns_number_total             14937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9000736sup3.cif
_cod_data_source_block           Eu123K
_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.

'_exptl_absorpt_correction_type' value 'multi scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' 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      'C2/c  '
_cod_database_code               4509449