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_4345224
_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         '2(C20 H16 Cu N4), O40 Si W12, 2(O)'
_chemical_formula_sum            'C40 H32 Cu2 N8 O42 Si W12'
_chemical_formula_weight         3658.11
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2bc 2ac'
_space_group_name_H-M_alt        'P c a b'
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1442(8)
_cell_length_b                   18.3980(7)
_cell_length_c                   20.6284(10)
_cell_measurement_reflns_used    4295
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.290
_cell_measurement_theta_min      2.573
_cell_volume                     6506.6(5)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    21.878
_exptl_absorpt_correction_T_max  0.2735
_exptl_absorpt_correction_T_min  0.1379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.533
_refine_diff_density_min         -2.187
_refine_diff_density_rms         0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.394
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         5738
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.366
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.000
_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^+1009.4089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1851
_reflns_number_gt                4814
_reflns_number_total             5738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02601_si_002.cif
_cod_data_source_block           p5
_cod_depositor_comments
'Adding full bibliography for 4345220--4345224.cif.'
_cod_database_code               4345224
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.00001 and
sigma for terminal atoms of 0.00001
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.00001 and
sigma for terminal atoms of 0.00001
Uanis(O9) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(O22) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.2
Uanis(O22) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.2
3. Others
 Fixed Sof: O11(0.5) O14(0.5) O18(0.5) O19(0.5)
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), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'