Crystal Structure and Band Gap Engineering in Polyoxometalate-Based Inorganic-Organic Hybrids.
Roy, Soumyabrata; Sarkar, Sumanta; Pan, Jaysree; Waghmare, Umesh V.; Dhanya, R.; Narayana, Chandrabhas; Peter, Sebastian C.; Inorganic chemistry 55 (2016) 3364–3377; doi:10.1021/acs.inorgchem.5b02718

data_4347092
_publ_section_title
;
 Crystal Structure and Band Gap Engineering in Polyoxometalate-Based
 Inorganic-Organic Hybrids.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3364
_journal_page_last               3377
_journal_paper_doi               10.1021/acs.inorgchem.5b02718
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'Mo12 O40 Si, 2(H2 O), C30 H24 Cl2 Cu3 N6, C20 H16 Cu2 N4'
_chemical_formula_sum            'C50 H44 Cl2 Cu5 Mo12 N10 O42 Si'
_chemical_formula_weight         3024.92
_chemical_name_common            '[(SiMo12O40)][Cu5Cl2(C10H8N2)5].2H2O'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_cell_angle_alpha                85.513(8)
_cell_angle_beta                 82.560(9)
_cell_angle_gamma                63.280(12)
_cell_formula_units_Z            2
_cell_length_a                   13.9658(17)
_cell_length_b                   14.2231(16)
_cell_length_c                   21.732(2)
_cell_measurement_reflns_used    13467
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.8
_cell_volume                     3822.4(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Smart X2 APEX II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28360
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.806
_exptl_absorpt_coefficient_mu    3.439
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_description       block
_exptl_crystal_F_000             2894
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         13467
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.0969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+44.5203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.2082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6776
_reflns_number_total             13467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02718_si_005.cif
_cod_data_source_block           sbr_017_001
_cod_original_cell_volume        3822.3(8)
_cod_database_code               4347092
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C27 \\sim N4: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3.a Free rotating group:
 O41(H41A,H41B), O42(H42A,H42B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50)
;
_shelx_res_checksum              50832
_shelx_hkl_checksum              33431
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'