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_7225282
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-26 deposited with the CCDC.
2016-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                63.169(3)
_cell_angle_beta                 71.079(3)
_cell_angle_gamma                63.827(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8897(4)
_cell_length_b                   14.0070(5)
_cell_length_c                   15.3382(4)
_cell_measurement_reflns_used    15926
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28.7490
_cell_measurement_theta_min      1.8290
_cell_volume                     2190.49(14)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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_environment      N~2~
_diffrn_ambient_temperature      125(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 0.915
_diffrn_measurement_details
;
  1 omega   84.00  118.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -       27.2058  178.0000   60.0000 34

  2 omega   70.00  116.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -       27.2058  178.0000  -90.0000 46

  3 omega -115.00  -73.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871  178.0000  -60.0000 42

  4 omega  -35.00   52.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871   37.0000  150.0000 87

  5 omega  -49.00   51.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871   37.0000   60.0000 100

  6 omega  -99.00   -7.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871  -57.0000 -180.0000 92

  7 omega  -86.00   -1.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871  -37.0000 -120.0000 85

  8 omega  -41.00    2.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -       27.2058  126.0000 -128.3268 43

  9 omega -102.00  -14.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871  -57.0000  150.0000 88

 10 omega  -49.00   52.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871   37.0000 -180.0000 101

 11 omega -108.00   13.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871  -77.0000  -60.0000 121

 12 omega  -49.00   52.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871   37.0000  -30.0000 101

 13 omega -108.00   13.00   1.0000   11.4750
omega____ theta____ kappa____ phi______ frames
    -      -27.9871  -77.0000   60.0000 121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0479045000
_diffrn_orient_matrix_UB_12      -0.0459220000
_diffrn_orient_matrix_UB_13      -0.0109495000
_diffrn_orient_matrix_UB_21      -0.0027446000
_diffrn_orient_matrix_UB_22      0.0308188000
_diffrn_orient_matrix_UB_23      -0.0512141000
_diffrn_orient_matrix_UB_31      0.0393873000
_diffrn_orient_matrix_UB_32      0.0246741000
_diffrn_orient_matrix_UB_33      -0.0031779000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37397
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.882
_diffrn_reflns_theta_min         1.782
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    32.478
_exptl_absorpt_correction_T_max  0.099
_exptl_absorpt_correction_T_min  0.020
_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    4.988
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.4353
_exptl_crystal_size_mid          0.2037
_exptl_crystal_size_min          0.1372
_refine_diff_density_max         1.684
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.288
_refine_ls_extinction_coef       0.000185(9)
_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   1.154
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0183P)^2^+9.5779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9653
_reflns_number_total             10548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02088c2.cif
_cod_data_source_block           sb974_cu_siw_13_red_abs
_cod_depositor_comments
'Adding full bibliography for 7225280--7225283.cif.'
_cod_original_cell_volume        2190.49(15)
_cod_database_code               7225282
_chemical_oxdiff_formula         'Cu2 Si W12 O56'
_reflns_odcompleteness_completeness 100.00
_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'