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_7225283
_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'
_audit_creation_date             2016-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-14 deposited with the CCDC.
2016-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.432(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9010(3)
_cell_length_b                   22.1952(4)
_cell_length_c                   15.3468(3)
_cell_measurement_reflns_used    11581
_cell_measurement_temperature    123.7(6)
_cell_measurement_theta_max      28.7360
_cell_measurement_theta_min      1.8200
_cell_volume                     4381.27(16)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.7(6)
_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 0.993
_diffrn_measurement_details
;
  1 omega   26.00   60.00   1.0000   75.3900
omega____ theta____ kappa____ phi______ frames
    -       27.0496  -37.0000  120.0000 34

  2 omega  -11.00   17.00   1.0000   75.3900
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  -88.0000 -145.5107 28

  3 omega  -25.00   52.00   1.0000   75.3900
omega____ theta____ kappa____ phi______ frames
    -      -27.9089   37.0000   90.0000 77

  4 omega  -89.00    6.00   1.0000   75.3900
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  -57.0000  120.0000 95

  5 omega -112.00  -74.00   1.0000   75.3900
omega____ theta____ kappa____ phi______ frames
    -      -27.9089 -178.0000  -30.0000 38

  6 omega -102.00   -1.00   1.0000   75.3900
omega____ theta____ kappa____ phi______ frames
    -      -27.9089  -57.0000  -30.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0329989000
_diffrn_orient_matrix_UB_12      0.0173601000
_diffrn_orient_matrix_UB_13      0.0249395000
_diffrn_orient_matrix_UB_21      -0.0220772000
_diffrn_orient_matrix_UB_22      -0.0268583000
_diffrn_orient_matrix_UB_23      0.0156379000
_diffrn_orient_matrix_UB_31      0.0382404000
_diffrn_orient_matrix_UB_32      -0.0004131000
_diffrn_orient_matrix_UB_33      0.0357918000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.830
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    32.476
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.359
_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    4.987
_exptl_crystal_description       prism
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.2192
_exptl_crystal_size_mid          0.1508
_exptl_crystal_size_min          0.1283
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.295
_refine_ls_extinction_coef       0.000027(3)
_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   1.106
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9976
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+14.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8791
_reflns_number_total             9976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02088c2.cif
_cod_data_source_block           cusiw_3_210116_red_075_absent_re
_cod_depositor_comments
'Adding full bibliography for 7225280--7225283.cif.'
_cod_original_cell_volume        4381.25(16)
_cod_database_code               7225283
_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
;
1. Uiso/Uaniso restraints and constraints
Uanis(O21) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(O2) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'