Synthesis of a novel 3D supramolecular hybrid via in situ self-assembly for the degradation of organic dyes
Guo, Hong; Yu, Zhaoqiang; Su, Yajun; Jiang, Xin-Dong; Inorganica Chimica Acta 508 (2020) 119625–; doi:10.1016/j.ica.2020.119625

data_1564510
_publ_section_title
;
 Synthesis of a novel 3D supramolecular hybrid via in situ self-assembly
 for the degradation of organic dyes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119625
_journal_paper_doi               10.1016/j.ica.2020.119625
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         'O40 P W12, 4(C24 H16 Cl Cu N4)'
_chemical_formula_sum            'C96 H64 Cl4 Cu4 N16 O40 P W12'
_chemical_formula_weight         4714.76
_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
_cell_angle_alpha                70.283(19)
_cell_angle_beta                 73.998(19)
_cell_angle_gamma                79.183(19)
_cell_formula_units_Z            1
_cell_length_a                   14.797(7)
_cell_length_b                   16.179(8)
_cell_length_c                   16.859(7)
_cell_measurement_reflns_used    8028
_cell_measurement_temperature    293.15(2)
_cell_measurement_theta_max      27.641
_cell_measurement_theta_min      1.573
_cell_volume                     3632(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1607
_diffrn_reflns_av_unetI/netI     0.1524
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37675
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.641
_diffrn_reflns_theta_min         1.573
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    10.182
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_description       plate
_exptl_crystal_F_000             2159
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         9.449
_refine_diff_density_min         -7.452
_refine_diff_density_rms         0.452
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         16670
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.1247
_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^)+(0.1580P)^2^+166.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3258
_refine_ls_wR_factor_ref         0.3620
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11417
_reflns_number_total             16670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020_508-119625.cif
_cod_data_source_block           shelx_sq
_cod_database_code               1564510
_shelx_estimated_absorpt_t_max   0.235
_shelx_estimated_absorpt_t_min   0.235
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{W2, W2A}
{W5, W5A}
{W3A, W3}
{W6, W6A}
{O9, O9A}
3. Rigid bond restraints
 C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C16 \\sim C17 \\sim C3 \\sim C2 \\sim C19 \\sim C13: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C45) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C48) = Uanis(C45)
Uanis(O16) = Uanis(O10) = Uanis(O16) = Uanis(O8)
Uiso(W2) = Uiso(W2A)
Uiso(W5) = Uiso(W5A)
Uiso(W3) = Uiso(W3A)
Uiso(W6) = Uiso(W6A)
Uiso(O9) = Uiso(O9A)
5. Others
 Fixed Sof: W2(0.5) W3(0.5) W5(0.5) W6(0.5) O9(0.5) O4(0.5) O2(0.5) O3(0.5)
 O1(0.5) W2A(0.5) W5A(0.5) W3A(0.5) W6A(0.5) O9A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C15(H15), C14(H14), C13(H13), C34(H34), C4(H4), C6(H6),
 C29(H29), C10(H10), C25(H25), C33(H33), C20(H20), C32(H32), C26(H26), C21(H21),
  C1(H1), C22(H22), C27(H27), C9(H9), C30(H30), C3(H3), C42(H42), C8(H8),
 C45(H45), C46(H46), C44(H44), C2(H2), C41(H41), C38(H38), C39(H39), C37(H37)
6.b Fitted hexagon refined as free rotating group:
 C24(C23,C19,C17,C16,C18), C12(C7,C4,C6,C5,C11), C45(C46,N8,C47,C43,C44)
;
_shelx_res_checksum              60547
_shelx_hkl_checksum              98257
_shelx_fab_checksum              3896