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_4347889
_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 Ge12 O64 Sm8, 14(O)'
_chemical_formula_sum            'C36 H108 Ge12 O78 Sm8'
_chemical_formula_weight         3863.10
_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                 100.916(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3203(4)
_cell_length_b                   23.4821(7)
_cell_length_c                   15.9302(5)
_cell_measurement_reflns_used    13111
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4768
_cell_measurement_theta_min      2.8967
_cell_volume                     4892.6(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0923
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25877
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_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    8.453
_exptl_absorpt_correction_T_max  0.4303
_exptl_absorpt_correction_T_min  0.2264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.812
_refine_diff_density_min         -3.578
_refine_diff_density_rms         0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     3007
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1216P)^2^+91.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                7479
_reflns_number_total             8591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00754_si_004.cif
_cod_data_source_block           exp_6734
_cod_original_cell_volume        4892.6(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4347889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Restrained distances
 O12W-O13W
 3 with sigma of 0.01
 C2'-C3 = C5'-C6 = C8'-C9 = C11'-C12 = C14'-C15 = C17'-C18
 1.43 with sigma of 0.01
 C1'-C2' = C4'-C5' = C7'-C8' = C10'-C11' = C13'-C14' = C16'-C17'
 1.5 with sigma of 0.01
 C2-C3 = C5-C6 = C8-C9 = C11-C12 = C14-C15 = C17-C18
 1.43 with sigma of 0.01
 C1-C2 = C4-C5 = C7-C8 = C10-C11 = C13-C14 = C16-C17
 1.5 with sigma of 0.01
 Ge1-C3 = Ge2-C6 = Ge3-C9 = Ge4-C12 = Ge5-C15 = Ge6-C18
 1.94 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C7) = Uanis(C4')
Uanis(C10) = Uanis(C7')
Uanis(C13) = Uanis(C10')
Uanis(O3W) = Uanis(O14')
Uanis(O14) = Uanis(O3W')
4. Others
 Sof(O13')=Sof(O14')=Sof(O3W')=Sof(C1')=Sof(C2')=Sof(C4')=Sof(C5')=Sof(C7')=
 Sof(C8')=Sof(C10')=Sof(C11')=Sof(C13')=Sof(C14')=Sof(C16')=Sof(C17')=1-FVAR(1)
 Sof(O13)=Sof(O14)=Sof(O3W)=Sof(C1)=Sof(C2)=Sof(C4)=Sof(C5)=Sof(C7)=Sof(C8)=
 Sof(C10)=Sof(C11)=Sof(C13)=Sof(C14)=Sof(C16)=Sof(C17)=FVAR(1)
 Fixed Sof: Ge4(0.5) Ge4'(0.5)
5.a Riding coordinates:
 O1W(H1A,H1B), O2W(H2A,H2B), O4W(H4A,H4B), O5W(H5A,H5B), O6W(H6A,H6B), O7W(H7A,
 H7B), O8W(H8A,H8B)
;
_olex2_submission_special_instructions 'No special instructions were received'