Lanthanide Germanate Cluster Organic Frameworks Based on {Ln8Ge12} Clusters: From One-Dimensional Chains to Two-Dimensional Layers and Three-Dimensional Frameworks.
Li, Lei-Lei; Cao, Gao-Juan; Zhao, Jun-Wei; He, Huan; Yang, Bai-Feng; Yang, Guo-Yu; Inorganic chemistry 55 (2016) 5671–5683; doi:10.1021/acs.inorgchem.6b00754

data_4347892
_publ_section_title
;
 Lanthanide Germanate Cluster Organic Frameworks Based on {Ln8Ge12}
 Clusters: From One-Dimensional Chains to Two-Dimensional Layers and
 Three-Dimensional Frameworks.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5671
_journal_page_last               5683
_journal_paper_doi               10.1021/acs.inorgchem.6b00754
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H28 Eu8 Ge12 O64, 14(O)'
_chemical_formula_sum            'C36 H108 Eu8 Ge12 O78'
_chemical_formula_weight         3875.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.913(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2863(2)
_cell_length_b                   23.4503(4)
_cell_length_c                   15.9547(3)
_cell_measurement_reflns_used    14686
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3906
_cell_measurement_theta_min      2.8077
_cell_volume                     4881.07(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33515
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    8.800
_exptl_absorpt_correction_T_max  0.4182
_exptl_absorpt_correction_T_min  0.2477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.823
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         10894
_refine_ls_number_restraints     2676
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+68.2235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                8765
_reflns_number_total             10894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00754_si_005.cif
_cod_data_source_block           exp_4
_cod_original_cell_volume        4881.07(14)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4347892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C2' \\sim C3 \\sim C3' \\sim C4 \\sim C5 \\sim C5' \\sim C6
\\sim C6' \\sim C7 \\sim C8 \\sim C8' \\sim C9 \\sim C10 \\sim C11 \\sim C11'
\\sim C12 \\sim C12' \\sim C13 \\sim C14 \\sim C14' \\sim C15 \\sim C15' \\sim
C16 \\sim C17 \\sim C17' \\sim C18 \\sim C18' \\sim C9' \\sim O1 \\sim O1W
\\sim O2 \\sim O2W \\sim O3 \\sim O3W \\sim O4 \\sim O4W \\sim O5 \\sim O5W
\\sim O6 \\sim O6W \\sim O7 \\sim O7W \\sim O8 \\sim O9 \\sim O10 \\sim O11
\\sim O12 \\sim O13 \\sim O13' \\sim O14 \\sim O14' \\sim O15 \\sim O15' \\sim
O16 \\sim O16' \\sim O17 \\sim O17' \\sim O18 \\sim O18' \\sim O19 \\sim O20
\\sim O20' \\sim O21 \\sim O21' \\sim O22 \\sim O22' \\sim O23 \\sim O23' \\sim
O24 \\sim O24' \\sim O8W \\sim O8W' \\sim O15W \\sim O13W \\sim O14W \\sim O12W
\\sim O11W \\sim O10W \\sim O9W: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O20) \\sim Ueq, Uanis(O20') \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O9W)
\\sim Ueq, Uanis(O10W) \\sim Ueq, Uanis(O13W) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
3. Others
 Sof(C2')=Sof(C3')=Sof(C5')=Sof(C6')=Sof(C8')=Sof(C11')=Sof(C12')=Sof(O13')=
 Sof(C14')=Sof(O14')=Sof(C15')=Sof(O15')=Sof(O16')=Sof(C17')=Sof(O17')=
 Sof(C18')=Sof(O18')=Sof(O20')=Sof(O21')=Sof(O22')=Sof(O23')=Sof(O24')=
 Sof(O8W')=Sof(C9')=1-FVAR(1)
 Sof(C2)=Sof(C3)=Sof(C5)=Sof(C6)=Sof(C8)=Sof(C9)=Sof(C11)=Sof(C12)=Sof(O13)=
 Sof(C14)=Sof(O14)=Sof(C15)=Sof(O15)=Sof(O16)=Sof(C17)=Sof(O17)=Sof(C18)=
 Sof(O18)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(O23)=Sof(O24)=Sof(O8W)=FVAR(1)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,
 H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB)
;
_olex2_submission_special_instructions 'No special instructions were received'