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_1560239
_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         'C34 H20 Br2 N4 O4, C16 H32 O8'
_chemical_formula_sum            'C50 H52 Br2 N4 O12'
_chemical_formula_weight         1060.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-24
_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                90
_cell_angle_beta                 105.93(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.889(5)
_cell_length_b                   18.209(4)
_cell_length_c                   33.691(7)
_cell_measurement_reflns_used    3221
_cell_measurement_temperature    170
_cell_measurement_theta_max      39.5090
_cell_measurement_theta_min      2.3380
_cell_volume                     11733(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      3.93  97.53   1.80   10.00    --   20.69  59.25 159.92   52
  2  \f   -349.73   8.47   1.80   40.00 -80.41 -89.16 -31.50    --   199
  3  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74  10.05   56
  4  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74-149.95   56
  5  \w      3.93  97.53   1.80   10.00    --   20.69  59.25-110.08   52
  6  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74 130.05   56
  7  \w    -26.23  70.97   1.80   15.00    --   50.69 -83.74  29.95   54
  8  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74 -29.95   56
  9  \w    192.04 285.64   1.80   40.00    --  -89.16 -59.25 -99.92   52
 10  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74  90.05   56
 11  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74-109.95   56
 12  \w    192.04 285.64   1.80   40.00    --  -89.16 -59.25 140.08   52
 13  \w    192.04 285.64   1.80   40.00    --  -89.16 -59.25-139.92   52
 14  \w   -120.80 -20.00   1.80   40.00    --  -89.16  83.74  50.05   56
;
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0167089000
_diffrn_orient_matrix_UB_12      0.0505910000
_diffrn_orient_matrix_UB_13      0.0330198000
_diffrn_orient_matrix_UB_21      -0.0708046000
_diffrn_orient_matrix_UB_22      -0.0379840000
_diffrn_orient_matrix_UB_23      -0.0062480000
_diffrn_orient_matrix_UB_31      0.0345058000
_diffrn_orient_matrix_UB_32      -0.0563311000
_diffrn_orient_matrix_UB_33      0.0336486000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.4617
_diffrn_reflns_av_unetI/netI     0.1686
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            111138
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        50.429
_diffrn_reflns_theta_max         50.429
_diffrn_reflns_theta_min         2.338
_diffrn_source                   'I\mS Microfocus Source'
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.350
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         12204
_refine_ls_number_restraints     1052
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.2789
_refine_ls_R_factor_gt           0.2005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4848
_refine_ls_wR_factor_ref         0.5352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5158
_reflns_number_total             12204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06837c2.cif
_cod_data_source_block           cu_uwdm_11_ligand
_cod_depositor_comments
'Adding full bibliography for 1560238--1560240.cif.'
_cod_database_code               1560239
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.666
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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 O(H) groups
2. Restrained distances
 C49B-C50B
 1.3 with sigma of 0.02
 C49A-C50A
 1.3 with sigma of 0.02
 O12-C49A
 1.5 with sigma of 0.02
 C6-C7
 1.4 with sigma of 0.002
 C28-C19
 1.4 with sigma of 0.002
 C16-C21
 1.4 with sigma of 0.002
 C1-C8
 1.4 with sigma of 0.002
 C89-C90
 1.4 with sigma of 0.002
 C95-C96
 1.4 with sigma of 0.002
 C99-C100
 1.4 with sigma of 0.002
 C81-C84
 1.4 with sigma of 0.002
 C24-C27
 1.4 with sigma of 0.002
 C31-C34
 1.4 with sigma of 0.002
 C51-C58
 1.4 with sigma of 0.002
 C62-C63
 1.4 with sigma of 0.002
 C66-C71
 1.4 with sigma of 0.002
 C69-C78
 1.4 with sigma of 0.002
 C74-C77
 1.4 with sigma of 0.002
 O12-C49B
 1.5 with sigma of 0.002
 C37-C38
 1.45 with sigma of 0.0002
3. Restrained planarity
 C34, H4, O4, O3, C31
 with sigma of 0.01
 H14, O14, C77, O13, C74
 with sigma of 0.01
 H16, O16, C84, O15, C81
 with sigma of 0.01
4. Rigid body (RIGU) restrains
 C55, Br3B, C53, C54, C52, C57, N5, C56, N6, C51, Br4B, C58, C59, C63, C60,
 C62, C61, C64, N8, N7, C70, C65, C69, C66, C78, C68, C71, C67, C79, C83, C72,
 C76, C80, C82, C73, C75, C81, C74, C84, C77, O16, O15, O14, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, Br2, C6, C7, C5, N1, C2, C1, C4, N2, C3, C8, Br1, C9, C13, C10, C12, C11,
  C14, N3, N4, C20, C15, C19, C16, C28, C18, C21, C17, C33, C29, C26, C22, C32,
 C30, C25, C23, C24, C34, C27, O3, O4, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C89, O17, C100, C85, C99, C86, O24, O18, C97, C87, O23, C88, C96, O19, C95,
 O22, C90, C94, O20, C93, C91, O21, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C45, O6, C36, C37, C35, C38, O5, O7, C50A, C50B, C39, C49A, C49B, C40, O12,
 O8, C48, C41, C47, C42, O11, O9, C46, C43, C44, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Br3B(0.5) Br4B(0.5) C50A(0.5) H50A(0.5) H50B(0.5) C49A(0.5)
 H49A(0.5) H49B(0.5) C49B(0.5) H49C(0.5) H49D(0.5) C50B(0.5) H50C(0.5)
 H50D(0.5) Br3A(0.5) Br4A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C92(H92A,H92B), C87(H87A,H87B), C38(H38A,
 H38B), C91(H91A,H91B), C93(H93A,H93B), C100(H10A,H10B), C41(H41A,H41B),
 C42(H42A,H42B), C88(H88A,H88B), C44(H44A,H44B), C47(H47A,H47B), C45(H45A,H45B),
  C85(H85A,H85B), C99(H99A,H99B), C35(H35A,H35B), C39(H39A,H39B), C43(H43A,
 H43B), C90(H90A,H90B), C94(H94A,H94B), C97(H97A,H97B), C46(H46A,H46B),
 C48(H48A,H48B), C50A(H50A,H50B), C96(H96A,H96B), C95(H95A,H95B), C89(H89A,
 H89B), C49A(H49A,H49B), C40(H40A,H40B), C86(H86A,H86B), C49B(H49C,H49D),
 C50B(H50C,H50D), C98(H98A,H98B)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1), N7(H7), C75(H75), C76(H76), C72(H72), C73(H73), C83(H83),
 C79(H79), C80(H80), C82(H82), C62(H62), C9(H9), C55(H55), C54(H54), C18(H18),
 C17(H17), C29(H29), C30(H30), C32(H32), C33(H33), C23(H23), C22(H22), C26(H26),
  C25(H25), N5(H5), C68(H68), C67(H67), C13(H13), C12(H12), C59(H59), C10(H10),
 C60(H60), C63(H63), C4(H4A), C5(H5A)
6.c Fitted hexagon refined as free rotating group:
 C74(C75,C76,C71,C72,C73), C83(C78,C79,C80,C81,C82), C57(C56,C55,C54,C53,C52),
 C16(C15,C20,C19,C18,C17), C28(C29,C30,C31,C32,C33), C24(C23,C22,C21,C26,C25),
 C66(C65,C70,C69,C68,C67)
6.d Tetrahedral OH refined with riding coordinates:
 O4(H4)
6.e Idealised tetrahedral OH refined as rotating group:
 O14(H14), O16(H16), O2(H2)
;
_shelx_res_checksum              15692
_shelx_hkl_checksum              1845
_shelx_fab_checksum              28974
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.759