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_4347094
_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
'2(Mo12 O40 Si), 5(C10 H8 Cu N2), 2(C10 H10 N2), 2(H2 O)'
_chemical_formula_sum            'C70 H64 Cu5 Mo24 N14 O82 Si2'
_chemical_formula_weight         5089.79
_chemical_name_common            '[H3(SiMo12O40)2][Cu5(C10H8N2)7].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                85.8030(10)
_cell_angle_beta                 88.4890(10)
_cell_angle_gamma                78.1060(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8950(3)
_cell_length_b                   13.5706(4)
_cell_length_c                   20.6833(6)
_cell_measurement_reflns_used    17227
_cell_measurement_temperature    293
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1.5
_cell_volume                     2984.18(15)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Smart X2 APEX II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44861
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        29.998
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.537
_exptl_absorpt_coefficient_mu    3.428
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.372
_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    2.832
_exptl_crystal_description       plate
_exptl_crystal_F_000             2419
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.811
_refine_diff_density_min         -2.469
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         17227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0630P)^2^+29.4147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10381
_reflns_number_total             17227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02718_si_002.cif
_cod_data_source_block           sbr001_in_p-1
_cod_database_code               4347094
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: O6(0.5) O14(0.5) O25(0.5) O35(0.5) O41(0.5) O42(0.5) O43(0.5)
 O44(0.5)
 Fixed X: HV(0.33729) HW(0.459449)
 Fixed Y: HV(0.160151) HW(0.17131)
 Fixed Z: HV(-0.14735) HW(-0.160531)
3.a Aromatic/amide H refined with riding coordinates:
 N6(H), N7(HA), C12(H12), C13(H13), C14(H14), C15(H15), C20(H20), C21(H21),
 C30(H30), C34(H34), C2(HB), C3(HC), C4(HD), C5(HE), C8(HF), C16(HG), C17(HH),
 C33(HI), C1(HJ), C7(HK), C19(HL), C35(HM), C22(HN), C23(HO), C25(HP), C26(HQ),
 C27(HR), C29(HS), C31(HT), C32(HU)
;
_shelx_res_checksum              23392
_shelx_hkl_checksum              90184
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'