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_4347093
_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 H10 N2)'
_chemical_formula_sum            'C20 H24 Cl0 Cu0 Mo12 N4 O42 Si'
_chemical_formula_weight         2171.80
_chemical_name_common            '[(H4SiMo12O40)][(C10H8N2)2].2H2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 103.319(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5292(4)
_cell_length_b                   12.0812(5)
_cell_length_c                   17.3184(7)
_cell_measurement_reflns_used    4087
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.6
_cell_volume                     2347.34(16)
_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      295.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Smart X2 APEX II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23967
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.567
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dull yellowish green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.073
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0789
_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^)+64.6160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3176
_reflns_number_total             4087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02718_si_004.cif
_cod_data_source_block           sbr105
_cod_database_code               4347093
_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: O3(0.5) O16(0.5) O19(0.5) O20(0.5)
 Fixed X: H(WA(0.61904) H(WB(0.57712)
 Fixed Y: H(WA(0.19603) H(WB(0.15007)
 Fixed Z: H(WA(0.035029) H(WB(0.096849)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9),
 C10(H10)
;
_shelx_res_checksum              40939
_shelx_hkl_checksum              77794
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'