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_4123526
_publ_section_title
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 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_formula_moiety
'2(C42 H70 O35), Mo12 O40 P, La H18 O9, 27(O)'
_chemical_formula_sum            'C84 H158 La Mo12 O146 P'
_chemical_formula_weight         4825.25
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2013-08-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.763(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2351(7)
_cell_length_b                   42.456(2)
_cell_length_c                   15.4011(7)
_cell_measurement_reflns_used    9108
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.35
_cell_volume                     9752.6(8)
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.04
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            161017
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         0.96
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0835 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.9332.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             4812
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.063
_refine_diff_density_max         4.781
_refine_diff_density_min         -2.482
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details
;
 Flack x determined using 16687 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.031(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2250
_refine_ls_number_reflns         39978
_refine_ls_number_restraints     2271
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+16.2099P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                36606
_reflns_number_total             39978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511713c_si_003.cif
_cod_data_source_block           n2964
_cod_depositor_comments
'Adding full bibliography for 4123525--4123526.cif.'
_cod_original_cell_volume        9752.5(8)
_cod_database_code               4123526
_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, All O(H,H) groups
2. Restrained distances
 O118-H11Q
 0.86 with sigma of 0.001
 O118-H11P
 0.86 with sigma of 0.001
 H11Q-H11P
 1.67 with sigma of 0.01
 La1-H11P
 3.1 with sigma of 0.1
 H11Q-La1
 3.1 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Rotating group:
 O111(H11B,H11C), O112(H11D,H11E), O113(H11F,H11G), O114(H11H,H11I), O115(H11J,
 H11K), O116(H11L,H11M), O117(H11N,H11O), O119(H11R,H11S)
4.b Ternary CH refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4A), C5(H5), C7(H7A), C8(H8), C9(H9A), C10(H10),
  C11(H11A), C13(H13), C14(H14A), C15(H15), C16(H16A), C17(H17A), C19(H19A),
 C20(H20), C21(H21A), C22(H22A), C23(H23), C25(H25), C26(H26A), C27(H27A),
 C28(H28), C29(H29A), C31(H31A), C32(H32A), C33(H33), C34(H34A), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44A),
 C45(H45), C46(H46A), C47(H47A), C49(H49A), C50(H50), C51(H51A), C52(H52A),
 C53(H53), C55(H55), C56(H56A), C57(H57A), C58(H58), C59(H59A), C61(H61A),
 C62(H62A), C63(H63), C64(H64A), C65(H65), C67(H67A), C68(H68), C69(H69A),
 C70(H70), C71(H71), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C79(H79),
  C80(H80), C81(H81), C82(H82), C83(H83)
4.c 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), C54(H54A,H54B), C60(H60A,H60B),
  C66(H66A,H66B), C72(H72A,H72B), C78(H78A,H78B), C84(H84A,H84B)
4.d Tetrahedral OH refined with riding coordinates:
 O6(H6), O19(H19), O69(H69)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O4(H4), O7(H7), O9(H9), O11(H11), O12(H12), O14(H14),
 O16(H16), O17(H17), O21(H21), O22(H22), O24(H24), O26(H26), O27(H27), O29(H29),
  O31(H31), O32(H32), O34(H34), O36(H36), O37(H37A), O39(H39A), O41(H41A),
 O42(H42), O44(H44), O46(H46), O47(H47), O49(H49), O51(H51), O52(H52), O54(H54),
  O56(H56), O57(H57), O59(H59), O61(H61), O62(H62), O64(H64), O66(H66), O67(H67)
;
_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 = 2148.3 Ang^3^ [22.0%]
Total electron count / cell = 370.5
;
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.842
_shelx_hkl_checksum              93114
_shelx_res_checksum              1475
_shelxl_version_number           2012-9