Disorder and polymorphism in Cu(ii)-polyoxometalate complexes: [Cu1.5(H2O)7.5PW12O40]·4.75H2O, cis- & trans-[Cu2(H2O)10SiW12O40]·6H2O
Bajpe, Sneha R.; Henke, Sebastian; Lee, Jung-Hoon; Bristowe, Paul D.; Cheetham, Anthony K.; CrystEngComm 18 (2016) 5327–; doi:10.1039/C5CE02088C

data_7225281
_publ_section_title
;
 Disorder and polymorphism in Cu(ii)-polyoxometalate complexes:
 [Cu1.5(H2O)7.5PW12O40]&#x00B7;4.75H2O, cis- &amp;
 trans-[Cu2(H2O)10SiW12O40]&#x00B7;6H2O
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5327
_journal_paper_doi               10.1039/C5CE02088C
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'Cu2 O50 Si W12, 6(O)'
_chemical_formula_sum            'Cu2 H32 O56 Si W12'
_chemical_formula_weight         3289.62
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-02 deposited with the CCDC.
2016-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.527(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9789(6)
_cell_length_b                   22.2778(10)
_cell_length_c                   15.4690(5)
_cell_measurement_reflns_used    7851
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8450
_cell_measurement_theta_min      1.8110
_cell_volume                     4458.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
  1 omega  -15.00   15.00   1.0000  104.1100
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  -80.0000 -146.0772 30

  2 omega -102.00    1.00   1.0000  104.1100
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  -57.0000  -90.0000 103

  3 omega -118.00  -35.00   1.0000  104.1100
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  178.0000    0.0000 83

  4 omega  -14.00   46.00   1.0000  104.1100
omega____ theta____ kappa____ phi______ frames
    -      -27.9089   37.0000   30.0000 60

  5 omega -108.00  -18.00   1.0000  104.1100
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  -37.0000   30.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0082907000
_diffrn_orient_matrix_UB_12      0.0309075000
_diffrn_orient_matrix_UB_13      0.0090171000
_diffrn_orient_matrix_UB_21      0.0406595000
_diffrn_orient_matrix_UB_22      -0.0075307000
_diffrn_orient_matrix_UB_23      0.0314732000
_diffrn_orient_matrix_UB_31      0.0358378000
_diffrn_orient_matrix_UB_32      0.0013525000
_diffrn_orient_matrix_UB_33      -0.0322912000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26186
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.061
_diffrn_reflns_theta_min         1.606
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    31.911
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    4.900
_exptl_crystal_description       plate
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.2839
_exptl_crystal_size_mid          0.1149
_exptl_crystal_size_min          0.0296
_refine_diff_density_max         3.304
_refine_diff_density_min         -2.804
_refine_diff_density_rms         0.485
_refine_ls_extinction_coef       0.000068(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8842
_reflns_number_total             10728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02088c2.cif
_cod_data_source_block           cu_siw_new_19_red_abs
_cod_depositor_comments
'Adding full bibliography for 7225280--7225283.cif.'
_cod_database_code               7225281
_chemical_oxdiff_formula         'Cu2 Si W12 O56 H32'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'