Probing Dynamic Library of Metal-Oxo Building Blocks with γ-Cyclodextrin.
Falaise, Clément; Moussawi, Mhamad Aly; Floquet, Sébastien; Abramov, Pavel A.; Sokolov, Maxim N.; Haouas, Mohamed; Cadot, Emmanuel; Journal of the American Chemical Society 140 (2018) 11198–11201; doi:10.1021/jacs.8b07525

data_4132940
_publ_section_title
;
 Probing Dynamic Library of Metal-Oxo Building Blocks with
 \g-Cyclodextrin.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11198
_journal_page_last               11201
_journal_paper_doi               10.1021/jacs.8b07525
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'O19 W6, C48 H56 O40, 13.5(O)'
_chemical_formula_sum            'C48 H56 O72.5 W6'
_chemical_formula_weight         2896.02
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.190(2)
_cell_length_b                   33.973(4)
_cell_length_c                   14.9308(18)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.49
_cell_volume                     9734.0(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            426898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         2.206
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.172
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1658 before and 0.1027 after correction. The Ratio of minimum to maximum transmission is 0.3835. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       plate
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.477
_refine_diff_density_min         -4.036
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.138(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         29842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+81.1780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                28051
_reflns_number_total             29842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07525_si_002.cif
_cod_data_source_block           cf53
_cod_original_cell_volume        9734(2)
_cod_original_formula_sum        'C48 H56 O72.50 W6'
_cod_database_code               4132940
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.314
_shelx_estimated_absorpt_t_min   0.121
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.862(9)
 0.138(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Others
 Fixed Sof: O8W(0.5) O3W(0.5) O2W(0.5)
4.a Ternary CH refined with riding coordinates:
 C34A(H34A), C30A(H30A), C8A(H8A), C33A(H33A), C14A(H14A), C7A(H7A), C3A(H3A),
 C20A(H20A), C46A(H46A), C29A(H29A), C27A(H27A), C43A(H43A), C36A(H36A),
 C2A(H2A), C25A(H25A), C35A(H35A), C13A(H13A), C24A(H24A), C22A(H22A),
 C42A(H42A), C12A(H12A), C32A(H32A), C37A(H37A), C18A(H18A), C21A(H21A),
 C11A(H11A), C38A(H38A), C10A(H10A), C48A(H48A), C16A(H16A), C17A(H17A),
 C41A(H41A), C47A(H47A), C23A(H23A), C44A(H44A), C40A(H40A), C28A(H28A),
 C1A(H1A), C5A(H5A), C4A(H4A)
4.b Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C45A(H45A,H45B), C26A(H26A,H26B), C6A(H6AA,H6AB), C15A(H15A,
 H15B), C9A(H9AA,H9AB), C39A(H39A,H39B), C19A(H19A,H19B)
;
_shelx_res_checksum              5890
_shelx_hkl_checksum              3466
_shelx_fab_checksum              58952
_olex2_submission_special_instructions 'No special instructions were received'