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_4345223
_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_absolute_configuration ad
_chemical_formula_moiety         '2(C30 H24 Co N6), Mo O40 Si W11, 8(O)'
_chemical_formula_sum            'C60 H48 Co2 Mo N12 O48 Si W11'
_chemical_formula_weight         3969.23
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                90.00
_cell_angle_beta                 119.695(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.024(7)
_cell_length_b                   13.347(3)
_cell_length_c                   24.530(5)
_cell_measurement_reflns_used    7015
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.501
_cell_measurement_theta_min      2.579
_cell_volume                     9108(3)
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23166
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.425
_exptl_absorpt_correction_T_max  0.3264
_exptl_absorpt_correction_T_min  0.1605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             7197
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         12846
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0400P)^2^+59.5303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                11169
_reflns_number_total             12846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02601_si_002.cif
_cod_data_source_block           p4
_cod_depositor_comments
'Adding full bibliography for 4345220--4345224.cif.'
_cod_database_code               4345223
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.914(11) 0.086(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
N4 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
C18 \\sim C19: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.08
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60)
;
_olex2_submission_special_instructions 'No special instructions were received'