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_7703008
_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
'Co4 Ge2 H4 Mo20 O74, C12 H36 Co3 N24 O6, 11(H2 O)'
_chemical_formula_sum            'C12 H62 Co7 Ge2 Mo20 N24 O91'
_chemical_formula_weight         4475.39
_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                110.550(4)
_cell_angle_beta                 98.559(4)
_cell_angle_gamma                112.651(4)
_cell_formula_units_Z            1
_cell_length_a                   13.9114(12)
_cell_length_b                   14.1874(12)
_cell_length_c                   14.6356(13)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.767
_cell_measurement_theta_min      3.414
_cell_volume                     2357.5(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31585
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.853
_diffrn_reflns_theta_max         66.853
_diffrn_reflns_theta_min         3.415
_exptl_absorpt_coefficient_mu    32.285
_exptl_absorpt_correction_T_max  0.002
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_colour_primary    'orange yellow'
_exptl_crystal_density_diffrn    3.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2123
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         8291
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0253P)^2^+9.8766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7085
_reflns_number_total             8380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04433g2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7703007--7703008.cif.'
_cod_database_code               7703008
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O10W) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(O7WA)=Sof(H7WC)=Sof(H7WD)=1-FVAR(1)
 Sof(O7W)=Sof(H7WA)=Sof(H7WB)=FVAR(1)
 Sof(O9WA)=Sof(H9WC)=Sof(H9WD)=1-FVAR(2)
 Sof(O9W)=Sof(H9WA)=Sof(H9WB)=FVAR(2)
 Fixed Sof: O10W(0.5) H10A(0.5) H10B(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O7WA(H7WC,
 H7WD), O8W(H8WA,H8WB), O9W(H9WA,H9WB), O9WA(H9WC,H9WD), O10W(H10A,H10B)
4.b Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C1(H1), C2(H2), C4(H4), C6(H6)
4.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B)
;
_shelx_res_checksum              5755
_olex2_submission_special_instructions 'No special instructions were received'