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_4132939
_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         'Mo6 O19, C48 H56 O40, 5.5(O)'
_chemical_formula_sum            'C48 H56 Mo6 O64.5'
_chemical_formula_weight         2240.56
_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     iterative
_audit_creation_date             2018-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.161(3)
_cell_length_b                   34.020(5)
_cell_length_c                   14.927(2)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    230
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.44
_cell_volume                     9730(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      230.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            123684
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.096
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         2.255
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1284 before and 0.0971 after correction. The Ratio of minimum to maximum transmission is 0.7852. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.287
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         17130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0584P)^2^+17.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                15646
_reflns_number_total             17130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07525_si_003.cif
_cod_data_source_block           testcf
_cod_original_cell_volume        9731(2)
_cod_original_formula_sum        'C48 H56 Mo6 O64.50'
_cod_database_code               4132939
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(4)
 0.03(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Others
 Fixed Sof: O5W(0.5) O7W(0.5) O2W(0.5) O1W(0.5) O3W(0.5) O4W(0.5) O8W(0.5)
 O6W(0.5) O9W(0.5)
4.a Ternary CH refined with riding coordinates:
 C3A(H3A), C9A(H9A), C1A(H1A), C26A(H26A), C2A(H2A), C22A(H22A), C25A(H25A),
 C28A(H28A), C42A(H42A), C16A(H16A), C34A(H34A), C40A(H40A), C17A(H17A),
 C19A(H19A), C10A(H10A), C21A(H21A), C33A(H33A), C8A(H8A), C41A(H41A),
 C37A(H37A), C13A(H13A), C31A(H31A), C23A(H23A), C14A(H14A), C29A(H29A),
 C20A(H20A), C11A(H11A), C32A(H32A), C6A(H6A), C27A(H27A), C7A(H7A), C47A(H47A),
  C45A(H45A), C35A(H35A), C44A(H44A), C46A(H46A), C43A(H43A), C5A(H5A),
 C15A(H15A), C38A(H38A)
4.b Secondary CH2 refined with riding coordinates:
 C24A(H24a,H24b), C36A(H36a,H36b), C39A(H39a,H39b), C12A(H12a,H12b), C30A(H30a,
 H30b), C4A(H4Aa,H4Ab), C18A(H18a,H18b), C48A(H48a,H48b)
;
_shelx_res_checksum              92902
_shelx_hkl_checksum              74894
_shelx_fab_checksum              91249
_olex2_submission_special_instructions 'No special instructions were received'