Reversible mechanical protection: building a 3D “suit” around a T-shaped benzimidazole axle
Zhu, Kelong; Baggi, Giorgio; Vukotic, V. Nicholas; Loeb, Stephen J.; Chem. Sci. 8 (2017) 3898–; doi:10.1039/C7SC00790F

data_1545989
_publ_section_title
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 Reversible mechanical protection: building a 3D &#x201C;suit&#x201D;
 around a T-shaped benzimidazole axle
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3898
_journal_paper_doi               10.1039/C7SC00790F
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C34 H50 O10, C25 H18 N2, 2(C H4 O)'
_chemical_formula_sum            'C61 H76 N2 O12'
_chemical_formula_weight         1029.23
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8421(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9848(10)
_cell_length_b                   19.3820(15)
_cell_length_c                   22.2953(17)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.24
_cell_volume                     5528.5(7)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0882
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.998
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7359
_exptl_absorpt_correction_T_min  0.5429
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1057 before and 0.0908 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         9760
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0597P)^2^+2.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6800
_reflns_number_total             9760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00790f2.cif
_cod_data_source_block           kz86m_0m
_cod_database_code               1545989
_shelx_shelxl_version_number     2016/4
_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, All O(H) groups
2. Same fragment restrains
{O7, O8A, C55A, C56A, C54A, C57} sigma for 1-2: 0.02, 1-3: 0.02
as
{O7, O8, C55, C56, C54, O8A}
3. Others
 Sof(O8A)=Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C56A)=Sof(H56C)=Sof(H56D)=
 Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(H57C)=Sof(H57D)=1-FVAR(1)
 Sof(O8)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=Sof(H57A)=Sof(H57B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C53(H53A,H53B), C48(H48A,H48B), C59(H59A,H59B), C52(H52A,
 H52B), C41(H41A,H41B), C47(H47A,H47B), C46(H46A,H46B), C42(H42A,H42B),
 C51(H51A,H51B), C38(H38A,H38B), C40(H40A,H40B), C50(H50A,H50B), C58(H58A,H58B),
  C49(H49A,H49B), C45(H45A,H45B), C43(H43A,H43B), C44(H44A,H44B), C55(H55A,
 H55B), C56(H56A,H56B), C54(H54A,H54B), C55A(H55C,H55D), C56A(H56C,H56D),
 C54A(H54C,H54D), C57(H57A,H57B), C57(H57C,H57D)
4.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C33(H33), C37(H37), C29(H29), C27(H27), C31(H31), C15(H15),
 C25(H25), C22(H22), C7(H7), C19(H19), C10(H10), C24(H24), C11(H11), C3(H3),
 C23(H23), C16(H16), C21(H21), C18(H18), C4(H4), C17(H17), C5(H5), C6(H6),
 N1(H1)
4.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
4.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S)
;
_olex2_submission_special_instructions 'No special instructions were received'