Translational dynamics of a non-degenerate molecular shuttle imbedded in a zirconium metal–organic framework
Wilson, Benjamin H.; Abdulla, Louae M.; Schurko, Robert W.; Loeb, Stephen J.; Chemical Science 12 (2021) 3944–3951; doi:10.1039/D0SC06837C

data_1560238
_publ_section_title
;
 Translational dynamics of a non-degenerate molecular shuttle imbedded in
 a zirconium metal--organic framework
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3944
_journal_page_last               3951
_journal_paper_doi               10.1039/D0SC06837C
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C38 H28 Br2 N4 O4, C16 H32 O8, C H4 O'
_chemical_formula_sum            'C55 H64 Br2 N4 O13'
_chemical_formula_weight         1148.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-12 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                75.171(4)
_cell_angle_beta                 83.247(4)
_cell_angle_gamma                84.427(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3936(9)
_cell_length_b                   16.7830(16)
_cell_length_c                   17.8687(17)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      50.33
_cell_measurement_theta_min      2.57
_cell_volume                     2697.7(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1374
_diffrn_reflns_av_unetI/netI     0.1289
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35147
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        50.895
_diffrn_reflns_theta_max         50.894
_diffrn_reflns_theta_min         2.570
_diffrn_source                   'I\mS Microfocus Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.464
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1425 before and 0.0860 after correction. The Ratio of minimum to maximum transmission is 0.7485. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.292
_refine_ls_R_factor_all          0.2112
_refine_ls_R_factor_gt           0.1520
_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^)+61.5421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3866
_reflns_number_total             5559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06837c2.cif
_cod_data_source_block           bhw319_1_0m
_cod_depositor_comments
'Adding full bibliography for 1560238--1560240.cif.'
_cod_database_code               1560238
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.791
_exptl_special_detail
;
Despite screening a number of crystals, all very small needles which resulted in weak diffraction.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C55 \\sim O13: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O13 \\sim C55: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
O10 \\sim C48: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C47 \\sim O9: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
3. Rigid body (RIGU) restrains
 Br1, Br2, O1, O2, O3, O4, N1, H1, N2, N3, H3, N4, C1, C2, C3, C4, H4, C5, H5,
 C6, C7, C8, C9, H9, C10, H10, C11, C12, H12, C13, H13, C14, C15, C16, C17, H17,
  C18, H18, C19, C20, C21, C22, H22, C23, H23, C24, C25, H25, C26, H26, C27,
 C28, H28A, H28B, C29, H29A, H29B, H29C, C30, C31, H31, C32, H32, C33, C34, H34,
  C35, H35, C36, C37, H37A, H37B, C38, H38A, H38B, H38C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
 C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C31(H31), C32(H32),
  C34(H34), C35(H35)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C55(H55A,H55B,H55C)
4.d Idealised tetrahedral OH refined as rotating group:
 O13(H13A)
;
_shelx_res_checksum              57650
_shelx_hkl_checksum              67794
_olex2_submission_special_instructions 'No special instructions were received'