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_7130971
_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         'C42 H49 Mn Mo9 Na3.05 O78'
_chemical_formula_sum            'C42 H49 Mn Mo9 Na3.05 O78'
_chemical_formula_weight         2790.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 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                   14.457(5)
_cell_length_b                   24.213(14)
_cell_length_c                   27.46(2)
_cell_measurement_reflns_used    9738
_cell_measurement_temperature    160
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.64
_cell_volume                     9612(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            77752
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         2.194
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1064 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.8676.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_description       block
_exptl_crystal_F_000             5446
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.602
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.192
_refine_ls_abs_structure_details
;
 Flack x determined using 8553 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         21773
_refine_ls_number_restraints     2064
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1190P)^2^+13.7414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1676
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                20261
_reflns_number_total             21773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05529e2.cif
_cod_data_source_block           q
_cod_database_code               7130971
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.873
_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
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C1B \\sim C2B \\sim
C3B \\sim C4B \\sim C5B \\sim C6B \\sim C1C \\sim C2C \\sim C3C \\sim C4C \\sim
C5C \\sim C6C \\sim C1D \\sim C2D \\sim C3D \\sim C4D \\sim C5D \\sim C6D \\sim
C1E \\sim C2E \\sim C3E \\sim C4E \\sim C5E \\sim C6E \\sim C1F \\sim C2F \\sim
C3F \\sim C4F \\sim C5F \\sim C6F \\sim C1G \\sim C2G \\sim C3G \\sim C4G \\sim
C5G \\sim C6G: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O1W
\\sim O2W \\sim O3W \\sim O4W \\sim O5W \\sim O6W \\sim O7W \\sim O8W \\sim O9W
\\sim O10W \\sim O11W \\sim O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim
O1B \\sim O2B \\sim O3B \\sim O4B \\sim O5B \\sim O1C \\sim O2C \\sim O3C \\sim
O4C \\sim O5C \\sim O1D \\sim O2D \\sim O3D \\sim O4D \\sim O5D \\sim O1E \\sim
O2E \\sim O3E \\sim O4E \\sim O5E \\sim O1F \\sim O2F \\sim O3F \\sim O4F \\sim
O5F \\sim O1G \\sim O2G \\sim O3G \\sim O4G \\sim O5G: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
3. Rigid body (RIGU) restrains
 C5C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: Na1(0.5) Na2(0.4) Na3(0.5) Na4(0.25) Na5(0.3) Na6(0.5) Na7(0.3)
 Na8(0.3)
5.a Ternary CH refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C1B(H1B), C2B(H2B),
 C3B(H3B), C4B(H4B), C5B(H5B), C1C(H1C), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C),
  C1D(H1D), C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D), C1E(H1E), C2E(H2E),
 C3E(H3E), C4E(H4E), C5E(H5E), C1F(H1F), C2F(H2F), C3F(H3F), C4F(H4F), C5F(H5F),
  C1G(H1G), C2G(H2G), C3G(H3G), C4G(H4G), C5G(H5G)
5.b Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C6B(H6BA,H6BB), C6C(H6CA,H6CB), C6D(H6DA,H6DB), C6E(H6EA,
 H6EB), C6F(H6FA,H6FB), C6G(H6GA,H6GB)
;
_shelx_res_checksum              3155
_shelx_hkl_checksum              64176
_olex2_submission_special_instructions 'No special instructions were received'