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_4347091
_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), 2(C10 H8 Cu N2), C10 H10 N2'
_chemical_formula_sum            'C30 H30 Cu2 Mo12 N6 O42 Si'
_chemical_formula_weight         2453.05
_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                105.1840(10)
_cell_angle_beta                 102.8070(10)
_cell_angle_gamma                114.8050(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8540(3)
_cell_length_b                   11.7897(3)
_cell_length_c                   13.2814(3)
_cell_measurement_reflns_used    7876
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.74
_cell_volume                     1378.15(6)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Smart X2 APEX II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28552
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.739
_exptl_absorpt_coefficient_mu    3.520
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.559
_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    2.956
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7876
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+10.6287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6401
_reflns_number_total             7876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02718_si_003.cif
_cod_data_source_block           sbr001redone
_cod_database_code               4347091
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
3. Others
 Fixed Sof: O17(0.5) O18(0.5) O21(0.5) O22(0.5)
 Fixed X: H23A(0.544499) H23B(0.528851)
 Fixed Y: H23A(0.182981) H23B(0.232659)
 Fixed Z: H23A(0.19486) H23B(0.111861)
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3A), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C14(H14), C15(H15)
;
_shelx_res_checksum              52390
_shelx_hkl_checksum              73421
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'