Complexation of polyoxometalates with cyclodextrins.
Wu, Yilei; Shi, Rufei; Wu, Yi-Lin; Holcroft, James M.; Liu, Zhichang; Frasconi, Marco; Wasielewski, Michael R.; Li, Hui; Stoddart, J. Fraser; Journal of the American Chemical Society 137 (2015) 4111–4118; doi:10.1021/ja511713c

data_4123525
_publ_section_title
;
 Complexation of polyoxometalates with cyclodextrins.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4111
_journal_page_last               4118
_journal_paper_doi               10.1021/ja511713c
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C48 H80 O40), (Mo12 O40 P), La O9'
_chemical_formula_sum            'C96 H160 La Mo12 O129 P'
_chemical_formula_weight         4699.39
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2013-08-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.5194(8)
_cell_length_b                   24.5275(8)
_cell_length_c                   18.4585(7)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      3.00
_cell_volume                     10648.2(6)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.05
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            76047
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.15
_diffrn_reflns_theta_min         1.80
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.026
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0813 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.6940.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.204
_refine_diff_density_max         2.385
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Flack x determined using 7596 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.072(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         18677
_refine_ls_number_restraints     2955
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0860
_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^)+(0.1454P)^2^+73.0447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2374
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                17642
_reflns_number_total             18677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511713c_si_002.cif
_cod_data_source_block           n2891c
_cod_depositor_comments
'Adding full bibliography for 4123525--4123526.cif.'
_cod_database_code               4123525
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 P1-O55 \\sim P1-O53 \\sim P1-O54 \\sim P1-O56
 with sigma of 0.02
 Mo1-O41 \\sim Mo2-O42 \\sim Mo3-O43 \\sim Mo4-O57 \\sim Mo5-O58 \\sim Mo6-O59 
 \\sim Mo7-O60 \\sim Mo8-O61
 \\sim Mo9-O62 \\sim Mo10-O75 \\sim Mo11-O76 \\sim Mo12-O77
 with sigma of 0.02
 Mo1-O44 \\sim Mo2-O44 \\sim Mo2-O45 \\sim Mo3-O45 \\sim Mo3-O46 \\sim Mo1-O46 
 \\sim Mo1-O47 \\sim Mo2-O48
 \\sim Mo2-O49 \\sim Mo3-O50 \\sim Mo3-O51 \\sim Mo1-O52 \\sim Mo4-O47 
 \\sim Mo4-O64 \\sim Mo5-O64 \\sim Mo5-
 O48 \\sim Mo5-O65 \\sim Mo6-O65 \\sim Mo6-O49 \\sim Mo6-O66 \\sim Mo7-O66 
 \\sim Mo7-O50 \\sim Mo7-O67 -
 Mo8-O67 \\sim Mo8-O51 \\sim Mo8-O68 \\sim Mo9-O68 \\sim Mo9-O52 \\sim Mo9-O63 
 \\sim Mo4-O63 \\sim Mo4-O69
 \\sim Mo10-O69 \\sim Mo10-O70 \\sim Mo5-O70 \\sim Mo6-O71 \\sim Mo11-O71 
 \\sim Mo10-O78 \\sim Mo11-O78 -
 Mo11-O72 \\sim Mo7-O72 \\sim Mo11-O79 \\sim Mo12-O79 \\sim Mo12-O73 
 \\sim Mo12-O80 \\sim Mo10-O80 -
 Mo8-O73 \\sim Mo12-O74 \\sim Mo9-O74
 with sigma of 0.02
 Mo7-O55 \\sim Mo8-O55 \\sim Mo3-O55 \\sim Mo11-O56 \\sim Mo12-O56 
 \\sim Mo10-O56
 \\sim Mo9-O53 \\sim Mo1-
 O53 \\sim Mo4-O53 \\sim Mo2-O54 \\sim Mo5-O54 \\sim Mo6-O54
 with sigma of 0.02
 Mo1-Mo2 \\sim Mo2-Mo3 \\sim Mo3-Mo1 \\sim Mo10-Mo11 \\sim Mo11-Mo12 
 \\sim Mo12-Mo10
 with sigma of 0.02
 Mo4-Mo5 \\sim Mo5-Mo6 \\sim Mo6-Mo7 \\sim Mo7-Mo8 \\sim Mo8-Mo9 \\sim Mo9-Mo4
 with sigma of 0.02
 O57-O47 \\sim O57-O63 \\sim O57-O64 \\sim O57-O69
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O67) \\sim Ueq, Uanis(O65) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O68) 
\\sim Ueq, Uanis(O63) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O64) \\sim Ueq, 
Uanis(O58) \\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.003 and sigma for 
terminal atoms of 0.01
4. Others
 Fixed Sof: Mo1(0.5) Mo2(0.5) Mo3(0.5) Mo4(0.5) Mo5(0.5) Mo6(0.5) Mo7(0.5)
 Mo8(0.5) Mo9(0.5) Mo10(0.5) Mo11(0.5) Mo12(0.5) O41(0.5) O42(0.5) O43(0.5)
 O44(0.5) O45(0.5) O46(0.5) O47(0.5) O48(0.5) O49(0.5) O50(0.5) O51(0.5)
 O52(0.5) O53(0.5) O54(0.5) O55(0.5) O56(0.5) O57(0.5) O58(0.5) O59(0.5)
 O60(0.5) O61(0.5) O62(0.5) O63(0.5) O64(0.5) O65(0.5) O66(0.5) O67(0.5)
 O68(0.5) O69(0.5) O70(0.5) O71(0.5) O72(0.5) O73(0.5) O74(0.5) O75(0.5)
 O76(0.5) O77(0.5) O78(0.5) O79(0.5) O80(0.5)
 Fixed X: P1(1)
 Fixed Y: P1(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C5(H5A), C7(H7), C8(H8A), C9(H9A),
 C10(H10A), C11(H11), C13(H13A), C14(H14A), C15(H15A), C16(H16), C17(H17),
 C19(H19A), C20(H20A), C21(H21), C22(H22), C23(H23), C25(H25A), C26(H26),
 C27(H27), C28(H28A), C29(H29A), C31(H31), C32(H32), C33(H33A), C34(H34A),
 C35(H35A), C37(H37), C38(H38A), C39(H39A), C40(H40A), C41(H41), C43(H43),
 C44(H44), C45(H45), C46(H46), C47(H47)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B), C42(H42A,H42B), C48(H48A,H48B)
5.c Tetrahedral OH refined with riding coordinates:
 O3(H3), O5(H5), O13(H13)
5.d Tetrahedral OH refined as rotating group:
 O20(H20), O4(H4), O8(H8), O9(H9), O10(H10), O14(H14), O15(H15), O18(H18),
 O19(H19), O23(H23A), O24(H24), O25(H25), O28(H28), O29(H29), O30(H30),
 O33(H33), O34(H34), O35(H35), O38(H38), O39(H39), O40(H40)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 3520.8 Ang^3^ [33.1%]
Total electron count / cell = 964.3
;
_shelx_estimated_absorpt_t_max   0.291
_shelx_estimated_absorpt_t_min   0.167
_shelxl_version_number           2013-3