Crystal-to-crystal polymerisation of monosubstituted [PW<sub>11</sub>O<sub>39</sub>Cu(H<sub>2</sub>O)]<sup>5-</sup> Keggin-type anions.
Ruiz-Bilbao, Estibaliz; Pache, Aroa; Barrenechea, Unai; Reinoso, Santiago; San Felices, Leire; Vivanco, Maria dM; Lezama, Luis; Artetxe, Beñat; Gutiérrez-Zorrilla, Juan M; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9042–9051; doi:10.1039/d4dt00690a

data_7716021
_publ_section_title
;
 Crystal-to-crystal polymerisation of monosubstituted
 [PW<sub>11</sub>O<sub>39</sub>Cu(H<sub>2</sub>O)]<sup>5-</sup>
 Keggin-type anions.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9042
_journal_page_last               9051
_journal_paper_doi               10.1039/d4dt00690a
_journal_volume                  53
_journal_year                    2024
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Cu1 O39 P W11, C6 H4 Cu0.5 N O2, 5(C H6 N3)'
_chemical_formula_sum            'C11 H34 Cu1.5 N16 O41 P W11'
_chemical_formula_weight         3195.17
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-05-02 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.780(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0736(3)
_cell_length_b                   19.0786(6)
_cell_length_c                   20.5732(7)
_cell_measurement_reflns_used    14269
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.203
_cell_measurement_theta_min      2.072
_cell_measurement_wavelength     0.71073
_cell_volume                     5120.3(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
  1 omega   40.00  118.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767 -178.0000  150.0000 78

  2 omega  -40.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -19.0000  120.0000 133

  3 omega   11.00   80.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -99.0000 -120.0000 69

  4 omega   73.00  100.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   19.0000   30.0000 27

  5 omega   37.00   90.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000 -150.0000 53

  6 omega   66.00  110.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000  -90.0000 44

  7 omega   41.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000   90.0000 53

  8 omega  -32.00   35.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   19.0000   30.0000 67

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0327133
_diffrn_orient_matrix_UB_12      0.0285901
_diffrn_orient_matrix_UB_13      0.0064369
_diffrn_orient_matrix_UB_21      -0.0391422
_diffrn_orient_matrix_UB_22      -0.0148255
_diffrn_orient_matrix_UB_23      -0.0212723
_diffrn_orient_matrix_UB_31      -0.0188378
_diffrn_orient_matrix_UB_32      -0.018636
_diffrn_orient_matrix_UB_33      0.0264145
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Mo) X-ray micro-source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36597
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.561
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    25.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47538
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5650
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.2518
_exptl_crystal_size_min          0.2351
_refine_diff_density_max         7.727
_refine_diff_density_min         -4.213
_refine_diff_density_rms         0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         10054
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0740
_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^)+(0.0790P)^2^+476.9914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                7458
_reflns_number_total             10054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00690a2.cif
_cod_data_source_block           a2014166_ar624ht_100ktras165
_cod_depositor_comments
'Adding full bibliography for 7716020--7716022.cif.'
_cod_original_formula_sum        'C11 H34 Cu1.50 N16 O41 P W11'
_cod_database_code               7716021