Two Ni/Co-substituted sandwich-type germanomolybdates based on an unprecedented trivacant polyanion [α-GeMo<sub>10</sub>O<sub>36</sub>]<sup>8</sup>.
Xu, Hui; Liu, Xing-Man; Su, Tan; Chen, Wei-Chao; Su, Zhong-Min; Dalton transactions (Cambridge, England : 2003) 49 (2020) 977–982; doi:10.1039/c9dt04433g

data_7703007
_publ_section_title
;
 Two Ni/Co-substituted sandwich-type germanomolybdates based on an
 unprecedented trivacant polyanion
 [\a-GeMo<sub>10</sub>O<sub>36</sub>]<sup>8</sup>.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              977
_journal_page_last               982
_journal_paper_doi               10.1039/c9dt04433g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'Ge2 H4 Mo20 Ni4 O74, C12 H36 N24 Ni3 O6, 10(H2 O)'
_chemical_formula_sum            'C12 H60 Ge2 Mo20 N24 Ni7 O90'
_chemical_formula_weight         4455.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-28 deposited with the CCDC.	2019-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                110.716(2)
_cell_angle_beta                 98.574(2)
_cell_angle_gamma                112.773(2)
_cell_formula_units_Z            1
_cell_length_a                   13.9330(19)
_cell_length_b                   14.2147(19)
_cell_length_c                   14.591(2)
_cell_measurement_reflns_used    5368
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.259
_cell_measurement_theta_min      2.510
_cell_volume                     2351.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17517
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.322
_diffrn_reflns_theta_min         1.680
_exptl_absorpt_coefficient_mu    4.692
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale green'
_exptl_crystal_colour_primary    'pale green'
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         11563
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+1.8274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9154
_reflns_number_total             11710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04433g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7703007--7703008.cif.'
_cod_database_code               7703007
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.521
_shelx_estimated_absorpt_t_min   0.353
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1WA,H1WB} of O1W, {H5WA,H5WB} of O5W, All N(H,H) groups
 At 1.5 times of:
  {H2WA,H2WB} of O2W, {H3WA,H3WB} of O3W, {H10A,H10B} of O10W, {H6WA,H6WB} of
  O6W, {H8WA,H8WB} of O8W, {H9WA,H9WB} of O9W, {H4WA,H4WB} of O4W, {H7WA,H7WB}
  of O7W, {H7WC,H7WD} of O7WA
2. Uiso/Uaniso restraints and constraints
Uanis(O7W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7WA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O9W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O6W) \\sim Ueq, Uanis(O4W)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(O7WA)=Sof(H7WC)=Sof(H7WD)=1-FVAR(1)
 Sof(O7W)=Sof(H7WA)=Sof(H7WB)=FVAR(1)
 Fixed Sof: O8W(0.5) H8WA(0.5) H8WB(0.5) O9W(0.5) H9WA(0.5) H9WB(0.5)
4.a Riding coordinates:
 O10W(H10A,H10B), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O4W(H4WA,H4WB), O5W(H5WA,
 H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O7WA(H7WC,H7WD), O8W(H8WA,H8WB),
 O9W(H9WA,H9WB)
4.b Rotating group:
 O3W(H3WA,H3WB)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
4.d X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B)
;
_shelx_res_checksum              48380
_olex2_submission_special_instructions 'No special instructions were received'