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_7225280
_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         'Cu0.5 O42.5 P W12, Cu O5, 4.75(O)'
_chemical_formula_sum            'Cu1.5 H24.5 O52.25 P W12'
_chemical_formula_weight         3193.17
_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             2015-06-19
_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                90
_cell_angle_beta                 94.1800(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9417(2)
_cell_length_b                   21.8435(3)
_cell_length_c                   15.0559(2)
_cell_measurement_reflns_used    17019
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      28.7540
_cell_measurement_theta_min      1.8480
_cell_volume                     4244.86(10)
_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      123(1)
_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 0.926
_diffrn_measurement_details
;
  1 omega  -36.00  -10.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -       27.3621  129.0000 -149.1181 26

  2 omega -112.00  -45.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433  178.0000  120.0000 67

  3 omega -108.00   12.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433  -77.0000   30.0000 120

  4 omega  -38.00   46.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433   37.0000  -30.0000 84

  5 omega   57.00   99.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -       27.3621  178.0000  120.0000 42

  6 omega -102.00    7.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433  -57.0000   90.0000 109

  7 omega  -49.00   52.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433   37.0000  150.0000 101

  8 omega -119.00  -32.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433  178.0000  -30.0000 87

  9 omega -108.00   22.00   1.0000   14.0400
omega____ theta____ kappa____ phi______ frames
    -      -28.1433  -37.0000 -180.0000 130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0330340000
_diffrn_orient_matrix_UB_12      0.0098900000
_diffrn_orient_matrix_UB_13      -0.0327545000
_diffrn_orient_matrix_UB_21      0.0047911000
_diffrn_orient_matrix_UB_22      -0.0306567000
_diffrn_orient_matrix_UB_23      -0.0146856000
_diffrn_orient_matrix_UB_31      -0.0436663000
_diffrn_orient_matrix_UB_32      0.0041294000
_diffrn_orient_matrix_UB_33      -0.0306789000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            52136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.989
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    33.273
_exptl_absorpt_correction_T_max  0.050
_exptl_absorpt_correction_T_min  0.004
_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    4.997
_exptl_crystal_description       prism
_exptl_crystal_F_000             5556
_exptl_crystal_size_max          0.6557
_exptl_crystal_size_mid          0.3113
_exptl_crystal_size_min          0.1757
_refine_diff_density_max         4.649
_refine_diff_density_min         -2.107
_refine_diff_density_rms         0.321
_refine_ls_extinction_coef       0.000073(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   1.167
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0147P)^2^+69.2504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             10443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02088c2.cif
_cod_data_source_block           sb974_cu_hpw_vd_4_no_na_125k2_red_abs
_cod_depositor_comments
'Adding full bibliography for 7225280--7225283.cif.'
_cod_original_cell_volume        4244.85(11)
_cod_original_formula_sum        'Cu1.50 H24.50 O52.25 P W12'
_cod_database_code               7225280
_chemical_oxdiff_formula         'Cu1.5 P W12 O51.5'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 Cu2A-O46
 1.98 with sigma of 0.02
 Cu2A-O49A
 1.98 with sigma of 0.02
 Cu2A-O48A
 1.98 with sigma of 0.02
 Cu2A-O50A
 2.36 with sigma of 0.02
 Cu2A-O49B = Cu2A-O47A
 1.98 with sigma of 0.02
 Cu2B-O47B
 1.98 with sigma of 0.02
 Cu2B-O46
 1.98 with sigma of 0.02
 Cu2B-O49B
 1.98 with sigma of 0.001
 Cu2B-O48B
 1.98 with sigma of 0.02
 Cu2B-O50B
 2.36 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O52W) \\sim Ueq, Uanis(O51W) \\sim Ueq, Uanis(O53W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O48B) \\sim Ueq, Uanis(O48A) \\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(O47B)
\\sim Ueq, Uanis(O47A) \\sim Ueq, Uanis(O49B) \\sim Ueq, Uanis(O49A) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O50A) = Uanis(O50B)
Uanis(O48B) = Uanis(O48A) = Uanis(O49A) = Uanis(O47A) = Uanis(O46) =
Uanis(O49B) = Uanis(O47B)
3. Others
 Fixed Sof: Cu2A(0.25) Cu2B(0.25) O46(0.5) O47A(0.25) O47B(0.25) O48A(0.25)
 O48B(0.25) O49A(0.25) O49B(0.25) O50A(0.25) O50B(0.25) O51W(0.5) O52W(0.25)
 O53W(0.25) O57W(0.25) O58W(0.25) O59W(0.25)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'