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_1560240
_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 H29 Br2 N4 O4, B F4, C16 H32 O8, 0.5(C4 H10 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C57 H67.5 B Br2 F4 N4.5 O12.5'
_chemical_formula_weight         1262.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-12
_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                 106.34(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.49(2)
_cell_length_b                   10.505(4)
_cell_length_c                   43.418(18)
_cell_measurement_reflns_used    101844
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      65.084
_cell_measurement_theta_min      2.121
_cell_volume                     12470(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ApexIII
_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      170.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            98593
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'I\mS Microfocus Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1342 before and 0.0735 after correction. The Ratio of minimum to maximum transmission is 0.6596. 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    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             5216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.019
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1512
_refine_ls_number_reflns         21024
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.1139
_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^)+(0.1390P)^2^+90.5684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.3088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16902
_reflns_number_total             21024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06837c2.cif
_cod_data_source_block           bhw319_2_0m
_cod_depositor_comments
'Adding full bibliography for 1560238--1560240.cif.'
_cod_original_cell_volume        12468(12)
_cod_original_formula_sum        'C57 H67.50 B Br2 F4 N4.50 O12.50'
_cod_database_code               1560240
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.660
_shelx_estimated_absorpt_t_min   0.464
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C113-C114
 1.5 with sigma of 0.02
 C1A-C113
 1.5 with sigma of 0.02
 F7B-F5B
 2.29 with sigma of 0.02
 F5B-F6B
 2.29 with sigma of 0.02
 F5B-F8B
 2.29 with sigma of 0.02
 F8B-F6B
 2.29 with sigma of 0.02
 F6B-F7B
 2.29 with sigma of 0.02
 F7B-F8B
 2.29 with sigma of 0.02
 F5B-B2
 1.402 with sigma of 0.02
 C106-O24
 1.448 with sigma of 0.02
 C102-C101
 1.504 with sigma of 0.02
 C95-C96
 1.504 with sigma of 0.02
 O17-C108
 1.448 with sigma of 0.02
 O23-C105
 1.448 with sigma of 0.02
 O24-C106
 1.448 with sigma of 0.001
 O24-C107
 1.448 with sigma of 0.001
 C100-C99
 1.448 with sigma of 0.01
 C96-C95
 1.504 with sigma of 0.01
 C97-C98
 1.504 with sigma of 0.01
 C99-C100
 1.504 with sigma of 0.01
 C101-C102
 1.504 with sigma of 0.01
 C103-C104
 1.504 with sigma of 0.01
 C105-C106
 1.504 with sigma of 0.01
 C107-C108
 1.504 with sigma of 0.01
 O17-C93
 1.448 with sigma of 0.01
 O18-C94
 1.448 with sigma of 0.01
 O18-C95
 1.448 with sigma of 0.01
 O19-C97
 1.448 with sigma of 0.01
 O20-C98
 1.448 with sigma of 0.01
 O21-C101
 1.448 with sigma of 0.01
 O21-C100
 1.448 with sigma of 0.01
 C102-O22
 1.448 with sigma of 0.01
 O22-C103
 1.448 with sigma of 0.01
 O23-C104
 1.448 with sigma of 0.01
 C106-C107
 2.3 with sigma of 0.02
 C104-C105
 2.3 with sigma of 0.001
 O23-C106
 2.3 with sigma of 0.001
 C38-C37
 1.5 with sigma of 0.02
 C52-C51
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C28: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O2 \\sim C27 \\sim C28 \\sim C29: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C113 \\sim C114: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C113 \\sim C1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C28 \\sim C29: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C82 \\sim C83: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O14 \\sim C82: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O14 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C78 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O13 \\sim C81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C33 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O4 \\sim C37: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C37 \\sim C38: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O3 \\sim C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C91 \\sim C92: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 B2, F5A, F7A, F8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F5B, F6B, F7B, F8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, O7, O8, O9, O10, O11, O12, C39, C40, C41, C42, C43, C44, C45, C46,
 C47, C48, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, O18, O19, O20, O21, O22, O23, O24, C93, C94, C95, C96, C97, C98, C99,
 C100, C101, C102, C103, C104, C105, C106, C107, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C28, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H11H(0.4) H11I(0.4) H11F(0.6) H11G(0.6) C1A(0.6) H1AA(0.6)
 H1AB(0.6) H1AC(0.6) C114(0.4) H11J(0.4) H11K(0.4) H11L(0.4) F5A(0.6) F6A(0.6)
 F7A(0.6) F8A(0.6) F5B(0.4) F6B(0.4) F7B(0.4) F8B(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C37(H37A,H37B), C82(H82A,H82B), C91(H91A,H91B), 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), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J),
 C105(H10K,H10L), C106(H10M,H10N), C107(H10O,H10P), C108(H10Q,H10R), C111(H11A,
 H11B), C113(H11H,H11I), C113(H11F,H11G)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C4(H4A), 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), N5(H5A), N7(H7), N8(H8), C58(H58), C59(H59),
 C63(H63), C64(H64), C66(H66), C67(H67), C71(H71), C72(H72), C76(H76), C77(H77),
  C79(H79), C80(H80), C85(H85), C86(H86), C88(H88), C89(H89)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C83(H83A,H83B,H83C), C92(H92A,H92B,
 H92C), C112(H11C,H11D,H11E), C1A(H1AA,H1AB,H1AC), C114(H11J,H11K,H11L),
 C110(H11M,H11N,H11O)
;
_shelx_res_checksum              950
_shelx_hkl_checksum              21052
_shelx_fab_checksum              66509
_olex2_submission_special_instructions 'No special instructions were received'