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_7049020
_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, C6 H4 Cu0.5 Dy N O9, C18 H12 Cu2 N3 O8, C6 H4 Cu0.5 N O2, 7(O)'
_chemical_formula_sum            'C30 H52 Cu3 Dy Ge N5 O66 W12'
_chemical_formula_weight         4170.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.086(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.241(4)
_cell_length_b                   16.539(4)
_cell_length_c                   35.111(9)
_cell_measurement_reflns_used    4730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.955
_cell_measurement_theta_min      2.447
_cell_volume                     7570(4)
_computing_data_collection       'Bruker APEX2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            37973
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    20.455
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1664 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.3472.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            mazarine
_exptl_crystal_density_diffrn    3.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.647
_refine_diff_density_min         -2.712
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         13124
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                9046
_reflns_number_total             13124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt00312f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7049020--7049023.cif.'
_cod_original_cell_volume        7570(3)
_cod_database_code               7049020
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 W6-O1
 1.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(O27)
\\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O34) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: W5(0.95) W5'(0.05) W8(0.95) W8'(0.05) W12(0.95) W12'(0.05)
 Fixed Uiso: O13W(0.15858) O14W(0.1508) O15W(0.16819) O16W(0.16599)
5.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)
;
_olex2_submission_special_instructions 'No special instructions were received'