Supramolecular Hybrids of Chiral Waugh Polyoxometalate with Cyclodextrins
Qi, Zhen-Qing; Wang, Ming-Yue; Shen, Jia-Chi; Lan, YouZhao; Jiang, Zhan-Guo; Zhan, Cai-Hong; Chemical Communications  (2022) –; doi:10.1039/D2CC05529E

data_7130972
_publ_section_title
;
 Supramolecular Hybrids of Chiral Waugh Polyoxometalate with Cyclodextrins
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05529E
_journal_year                    2022
_chemical_formula_moiety         'C96 H112 Mn2 Mo18 Na5 O149, Mn Mo9 O32'
_chemical_formula_sum            'C96 H112 Mn3 Mo27 Na5 O181'
_chemical_formula_weight         7032.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2022-11-03 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.361(3)
_cell_length_b                   37.863(6)
_cell_length_c                   35.710(6)
_cell_measurement_reflns_used    9653
_cell_measurement_temperature    160.00
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.43
_cell_volume                     26178(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      160.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            96965
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.180
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             13600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.828
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.256
_refine_ls_abs_structure_details
;
 Flack x determined using 8695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.073(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1856
_refine_ls_number_reflns         29920
_refine_ls_number_restraints     2657
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1734P)^2^+88.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2292
_refine_ls_wR_factor_ref         0.2501
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                23148
_reflns_number_total             29920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05529e2.cif
_cod_data_source_block           222324_a_sq
_cod_original_cell_volume        26177(7)
_cod_database_code               7130972
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O10_2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Same fragment restrains
{Mn1_2, Mo1_2, Mo2_2, Mo3_2, Mo4_2, Mo5_2, Mo6_2, Mo7_2, Mo8_2, Mo9_2, O1_2,
O2_2, O3_2, O4_2, O5_2, O6_2, O7_2, O8_2, O9_2, O10_2, O11_2, O12_2, O13_2,
O14_2, O15_2, O16_2, O17_2, O18_2, O19_2, O20_2, O21_2, O22_2, O23_2, O24_2,
O25_2, O26_2, O27_2, O28_2, O29_2, O30_2, O31_2, O32_2}
{Mn1_3, Mo1_3, Mo2_3, Mo3_3, Mo4_3, Mo5_3, Mo6_3, Mo7_3, Mo8_3, Mo9_3, O1_3,
O2_3, O3_3, O4_3, O5_3, O6_3, O7_3, O8_3, O9_3, O10_3, O11_3, O12_3, O13_3,
O14_3, O15_3, O16_3, O17_3, O18_3, O19_3, O20_3, O21_3, O22_3, O23_3, O24_3,
O25_3, O26_3, O27_3, O28_3, O29_3, O30_3, O31_3, O32_3}
as
{Mn1_1, Mo1_1, Mo2_1, Mo3_1, Mo4_1, Mo5_1, Mo6_1, Mo7_1, Mo8_1, Mo9_1, O1_1,
O2_1, O3_1, O4_1, O5_1, O6_1, O7_1, O8_1, O9_1, O10_1, O11_1, O12_1, O13_1,
O14_1, O15_1, O16_1, O17_1, O18_1, O19_1, O20_1, O21_1, O22_1, O23_1, O24_1,
O25_1, O26_1, O27_1, O28_1, O29_1, O30_1, O31_1, O32_1} sigma for 1-2: 0.02
1-3: 0.04
4. Others
 Sof(Mn1)=Sof(Mo1)=Sof(Mo2)=Sof(Mo3)=Sof(Mo4)=Sof(Mo5)=Sof(Mo6)=Sof(Mo7)=
 Sof(Mo8)=Sof(Mo9)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=
 Sof(O8)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=
 Sof(O17)=Sof(O18)=Sof(O19)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(O23)=Sof(O24)=
 Sof(O25)=Sof(O26)=Sof(O27)=Sof(O28)=Sof(O29)=Sof(O30)=Sof(O31)=Sof(O32)=0.5*(1-
 FVAR(2))
 Sof(Mn1)=Sof(Mo1)=Sof(Mo2)=Sof(Mo3)=Sof(Mo4)=Sof(Mo5)=Sof(Mo6)=Sof(Mo7)=
 Sof(Mo8)=Sof(Mo9)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=
 Sof(O8)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=
 Sof(O17)=Sof(O18)=Sof(O19)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(O23)=Sof(O24)=
 Sof(O25)=Sof(O26)=Sof(O27)=Sof(O28)=Sof(O29)=Sof(O30)=Sof(O31)=Sof(O32)=0.5*
 FVAR(2)
 Fixed Sof: Na4(0.5) Na2(0.5) Na1(0.5)
 Fixed Y: Mn1(0.5)
 Fixed Z: Mn1(0.5)
5.a Free rotating group:
 Mo1(Mo2,Mo3,Mo4,Mo5,Mo6,Mo7,Mo8,Mo9,O1,O2,O3,O4,O5,O6,O7,O8,O9,O10,O11,O12,
 O13,O14,O15,O16,O17,O18,O19,O20,O21,O22,O23,O24,O25,O26,O27,O28,O29,O30,O31,
 O32)
5.b Ternary CH refined with riding coordinates:
 C2D(H2D), C4D(H4D), C1C(H1C), C3H(H3H), C4H(H4H), C1D(H1D), C2E(H2E),
 C4A(H4A), C2H(H2H), C4F(H4F), C1F(H1F), C2G(H2G), C2A(H2A), C3A(H3A), C3D(H3D),
  C3E(H3E), C3G(H3G), C1A(H1A), C5F(H5F), C5H(H5H), C5G(H5G), C1G(H1G),
 C1H(H1H), C2F(H2F), C1E(H1E), C2C(H2C), C4G(H4G), C5E(H5E), C1B(H1B), C5A(H5A),
  C5C(H5C), C4C(H4C), C3C(H3C), C4E(H4E), C5D(H5D), C3F(H3F), C4B(H4B),
 C2B(H2B), C3B(H3B), C5B(H5B)
5.c Secondary CH2 refined with riding coordinates:
 C6D(H6DA,H6DB), C6E(H6EA,H6EB), C6A(H6AA,H6AB), C6H(H6HA,H6HB), C6G(H6GA,
 H6GB), C6F(H6FA,H6FB), C6C(H6CA,H6CB), C6B(H6BA,H6BB)
;
_shelx_res_checksum              66493
_shelx_hkl_checksum              36751
_shelx_fab_checksum              36349
_olex2_submission_special_instructions 'No special instructions were received'