Organic-inorganic hybrid 1-D double chain heteropolymolybdates constructed from plenary Keggin germanomolybdate anions and hepta-nuclear Cu-RE-pic heterometallic clusters.
Hu, Huifen; Gong, Peijun; Pang, Jingjing; Jiang, Jun; Chen, Lijuan; Zhao, Junwei; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15977–15988; doi:10.1039/c9dt03083b

data_7701245
_publ_section_title
;
 Organic-inorganic hybrid 1-D double chain heteropolymolybdates
 constructed from plenary Keggin germanomolybdate anions and hepta-nuclear
 Cu-RE-pic heterometallic clusters.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15977
_journal_page_last               15988
_journal_paper_doi               10.1039/c9dt03083b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C60 H40 Cu5 Ge2 La2 Mo24 N10 O114, 2(N), 12(O)'
_chemical_formula_sum            'C60 H124 Cu5 Ge2 La2 Mo24 N12 O139'
_chemical_formula_weight         6280.96
_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     dual
_audit_creation_date             2019-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-07 deposited with the CCDC.    2019-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.4250(4)
_cell_length_b                   14.3964(3)
_cell_length_c                   28.9317(6)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.56
_cell_volume                     7930.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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      150.02
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60571
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.505
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1437 before and 0.0723 after correction. The Ratio 
of minimum to maximum transmission is 0.7933. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6022
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.38
_refine_diff_density_max         2.142
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.00014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         13899
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0455P)^2^+58.9580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11129
_reflns_number_total             13899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03083b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7701245--7701246.cif.'
_cod_database_code               7701245
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: La1(0.85) La1B(0.15) Mo1(0.75) Mo1B(0.25) Mo2(0.75) Mo2B(0.25)
 Mo3(0.75) Mo3B(0.25) Mo4(0.75) Mo4B(0.25) Mo6(0.75) Mo6B(0.25) Mo9(0.75)
 Mo9B(0.25)
 Fixed Uiso: O7W(0.05741) O8W(0.06)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28)
;
_shelx_res_checksum              46107
_shelx_fab_checksum              80309
_olex2_submission_special_instructions 'No special instructions were received'