Two Unprecedented POM-Based Inorganic-Organic Hybrids with Concomitant Heteropolytungstate and Molybdate.
Li, Yun-Wu; Guo, Ling-Yu; Su, Hai-Feng; Jagodič, Marko; Luo, Ming; Zhou, Xiao-Qi; Zeng, Su-Yuan; Tung, Chen-Ho; Sun, Di; Zheng, Lan-Sun; Inorganic chemistry 56 (2017) 2481–2489; doi:10.1021/acs.inorgchem.6b02601

data_4345221
_publ_section_title
;
 Two Unprecedented POM-Based Inorganic-Organic Hybrids with Concomitant
 Heteropolytungstate and Molybdate.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2481
_journal_page_last               2489
_journal_paper_doi               10.1021/acs.inorgchem.6b02601
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C48 H36 Cu6 Mo N18 O49 Si W12, 4(O)'
_chemical_formula_sum            'C48 H36 Cu6 Mo N18 O53 Si W12'
_chemical_formula_weight         4424.36
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                91.5050(10)
_cell_angle_beta                 106.5800(10)
_cell_angle_gamma                110.8050(10)
_cell_formula_units_Z            2
_cell_length_a                   13.35500(10)
_cell_length_b                   18.1021(2)
_cell_length_c                   20.3541(2)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.579
_cell_measurement_theta_min      2.432
_cell_volume                     4363.62(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41784
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.43
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.428
_exptl_absorpt_correction_T_max  0.2746
_exptl_absorpt_correction_T_min  0.1797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3982
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         7.757
_refine_diff_density_min         -4.202
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         15354
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0000P)^2^+170.3171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                12329
_reflns_number_total             15354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02601_si_002.cif
_cod_data_source_block           p2
_cod_depositor_comments
'Adding full bibliography for 4345220--4345224.cif.'
_cod_original_cell_volume        4363.61(7)
_cod_database_code               4345221
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
W10: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C37 \\sim C43: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
W10: within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.001
W10: within 1.7A with sigma of 0.0001 and sigma for terminal atoms of 0.0001
W10: within 1.7A with sigma of 0.00001 and sigma for terminal atoms of 0.00002
C36 \\sim C37: within 1.7A with sigma of 0.0001 and sigma for terminal atoms of
0.0002
C43 \\sim C44: within 1.7A with sigma of 0.0001 and sigma for terminal atoms of
0.0002
W9: within 1.7A with sigma of 0.00001 and sigma for terminal atoms of 0.00002
W10: within 1.7A with sigma of 0.000001 and sigma for terminal atoms of 0.000002
W9: within 1.7A with sigma of 0 and sigma for terminal atoms of 0
W9 \\sim O17: within 1.7A with sigma of 0.000001 and sigma for terminal atoms
of 0.000001
N15 \\sim C39 \\sim C40: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.08
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48)
;
_olex2_submission_special_instructions 'No special instructions were received'