Synthesis and PPy loading for enhanced visible-light photocatalytic activity of new POMOFs containing silver chains
Sha, Jing-Quan; Yang, Xi-Ya; Sheng, Ning; Liu, Guo-Dong; Li, Ji-Sen; Yang, Jian-Bo; Journal of Solid State Chemistry 263 (2018) 52–59; doi:10.1016/j.jssc.2018.04.008

data_1561053
_publ_section_title
;
 Synthesis and PPy loading for enhanced visible-light photocatalytic
 activity of new POMOFs containing silver chains
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              52
_journal_page_last               59
_journal_paper_doi               10.1016/j.jssc.2018.04.008
_journal_volume                  263
_journal_year                    2018
_chemical_formula_moiety         'C36 H36 Ag29 N54 O40 Si W12'
_chemical_formula_sum            'C36 H36 Ag29 N54 O40 Si W12'
_chemical_formula_weight         7227.71
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                77.670(5)
_cell_angle_beta                 67.997(5)
_cell_angle_gamma                69.991(5)
_cell_formula_units_Z            1
_cell_length_a                   12.934(5)
_cell_length_b                   15.925(5)
_cell_length_c                   16.164(5)
_cell_measurement_reflns_used    9033
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.430
_cell_measurement_theta_min      2.534
_cell_volume                     2886.6(17)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14528
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.37
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    16.779
_exptl_absorpt_correction_T_max  0.029
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3215
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         4.020
_refine_diff_density_min         -4.231
_refine_diff_density_rms         0.652
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         10048
_refine_ls_number_restraints     722
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.1260
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1045.6793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2948
_refine_ls_wR_factor_ref         0.2958
_reflns_number_gt                9527
_reflns_number_total             10048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2018-263-52.cif
_cod_data_source_block           dd
_cod_database_code               1561053
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(O) groups
2. Rigid bond restraints
 N3, N4, N17, C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, N7, N15, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, N10, N14, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N20, N21, N27, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N22, N23, N26, C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N12, N13, N16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, N18, N19, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, N11, N35, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim N17 \\sim C3 \\sim C4: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N5 \\sim N7 \\sim N15 \\sim C5 \\sim C6: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N2 \\sim N10 \\sim N14 \\sim C13 \\sim C14: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N20 \\sim N21 \\sim N27 \\sim C15 \\sim C16: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N22 \\sim N23 \\sim N26 \\sim C9 \\sim C10: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N12 \\sim N13 \\sim N16 \\sim C17 \\sim C18: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N1 \\sim N18 \\sim N19 \\sim C1 \\sim C2: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N6 \\sim N11 \\sim N35 \\sim C11 \\sim C12: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(N14) \\sim Ueq,
Uanis(N20) \\sim Ueq, Uanis(N24) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(N25) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N28) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Si1) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O16)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Ag16(0.5) Ag15(0.5) O8(0.5) O9(0.5) O11(0.5) O16(0.5)
5.a Riding coordinates:
 O9(O11)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'