Organic-inorganic hybrids assembled from plenary Keggin-type germanotungstate units and 3d-4f heterometal clusters.
Li, Huijie; Gong, Peijun; Jiang, Jun; Li, Yamin; Pang, Jingjing; Chen, Lijuan; Zhao, Junwei; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3730–3742; doi:10.1039/c9dt00312f

data_7049022
_publ_section_title
;
 Organic-inorganic hybrids assembled from plenary Keggin-type
 germanotungstate units and 3d-4f heterometal clusters.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3730
_journal_page_last               3742
_journal_paper_doi               10.1039/c9dt00312f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'Ge O40 W12, C18 H12 Cu2 La0.5 N3 Na0.5 O16, C18 H12 Cu2 N3 O8, 8(O)'
_chemical_formula_sum            'C36 H64 Cu4 Ge La0.5 N6 Na0.5 O72 W12'
_chemical_formula_weight         4346.83
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-02-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.9910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7617(9)
_cell_length_b                   14.7533(7)
_cell_length_c                   31.1104(15)
_cell_measurement_reflns_used    9539
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.988
_cell_measurement_theta_min      2.407
_cell_volume                     8578.6(7)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43205
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.694
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.4529.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            mazarine
_exptl_crystal_density_diffrn    3.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.419
_refine_diff_density_min         -2.842
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         15057
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0385P)^2^+149.0722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                11706
_reflns_number_total             15057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt00312f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7049020--7049023.cif.'
_cod_original_formula_sum        'C36 H64 Cu4 Ge La0.50 N6 Na0.50 O72 W12'
_cod_database_code               7049022
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{La1, Na1}
3. Restrained distances
 La1-O14W
 2.8 with sigma of 0.01
4. Rigid bond restraints
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(La1) = Uanis(Na1)
6. Others
 Fixed Sof: La1(0.5) Na1(0.5)
 Fixed Uiso: O3W(0.08902) O4W(0.08428) O5W(0.0863) O6W(0.08905) O7W(0.08352)
 O9W(0.09367) O14W(0.13141) O19W(0.14921) O45(0.05872)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C7(H7A), C8(H8A), C9(H9A), C10(H10A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C19(H19A), C20(H20A), C21(H21A),
 C22(H22A), C25(H25A), C26(H26A), C27(H27A), C28(H28A), C31(H31A), C32(H32A),
 C33(H33A), C34(H34A)
;
_olex2_submission_special_instructions 'No special instructions were received'