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_4347897
_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         '0.5(C104 H192 Ge28 Nd24 O168), 2(O)'
_chemical_formula_sum            'C52 H108 Ge14 Nd12 O90'
_chemical_formula_weight         4920.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7374(3)
_cell_length_b                   25.2703(4)
_cell_length_c                   27.2582(4)
_cell_measurement_reflns_used    23143
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5096
_cell_measurement_theta_min      2.8506
_cell_volume                     12217.9(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0517
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42182
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.86
_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    8.490
_exptl_absorpt_correction_T_max  0.4049
_exptl_absorpt_correction_T_min  0.2456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            PINK
_exptl_crystal_density_diffrn    2.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             9232
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;

;
_refine_diff_density_max         3.161
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     462
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0777P)^2^+713.1946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                9350
_reflns_number_total             10687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00754_si_009.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4347897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C23-C24 = C25-C26
 1.53 with sigma of 0.01
 C16-C17 = C17-C18 = C19-C20 = C20-C21
 1.53 with sigma of 0.05
 C1-C2 = C2-C3 = C4-C5 = C5-C6 = C7-C8 = C8-C9
 1.53 with sigma of 0.01
 C6-O16
 1.23 with sigma of 0.01
3. Rigid bond restraints
 O35, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq,
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq,
Uanis(O27) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30)
\\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq,
Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O1W)
\\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O5W) \\sim Ueq,
Uanis(O6W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O7W)
\\sim Ueq, : with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Others
 Fixed Sof: O14(0.5) O14'(0.5)
6.a Riding coordinates:
 O27(H27A), O1W(H1WB,H1WA), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WB,H5WA),
 O6W(H6WA,H6WB), O2W(H2WA,H2WB)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B)
6.c Aromatic/amide H refined with riding coordinates:
 O26(H26)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'