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_4345222
_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         'O40 Si W12, 4(C6 H8 Cu N4), 2(O)'
_chemical_formula_sum            'C24 H32 Cu4 N16 O42 Si W12'
_chemical_formula_weight         3705.11
_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             2016-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                66.182(13)
_cell_angle_beta                 83.004(15)
_cell_angle_gamma                65.199(13)
_cell_formula_units_Z            1
_cell_length_a                   12.73(2)
_cell_length_b                   13.22(2)
_cell_length_c                   13.85(2)
_cell_measurement_reflns_used    5239
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.474
_cell_measurement_theta_min      2.885
_cell_volume                     1932(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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16681
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.953
_exptl_absorpt_correction_T_max  0.2530
_exptl_absorpt_correction_T_min  0.1158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1642
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.707
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6704
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+23.9630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2184
_reflns_number_gt                4916
_reflns_number_total             6704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02601_si_002.cif
_cod_data_source_block           p3
_cod_depositor_comments
'Adding full bibliography for 4345220--4345224.cif.'
_cod_original_cell_volume        1932(6)
_cod_database_code               4345222
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
N3 \\sim N4: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
N5 \\sim C4 \\sim C5: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
N7 \\sim N8 \\sim C1 \\sim C2 \\sim C3: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: O5(0.5) O16(0.5) O17(0.5) O22(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), N5(H5),
 N8(H8A), C1(H1), C2(H2A), C3(H3), C4(H4A), C5(H5A), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'