Formation of an Interlocked Double-Chain from an Organic-Inorganic [2]Rotaxane
Ferrando-Soria, Jesus; Fernandez, Antonio; Vitorica-Yrzebal, Inigo; Asthana, Deepak; Muryn, Christopher; Tuna, Floriana; Timco, Grigore A.; Winpenny, Richard E. P.; Chemical Communications  (2019) –; doi:10.1039/C8CC09339C

data_7122958
_publ_section_title
;
 Formation of an Interlocked Double-Chain from an Organic-Inorganic
 [2]Rotaxane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09339C
_journal_year                    2019
_chemical_formula_moiety
'C80 H144 Cr7 F8 O32 Zn, C21 H22 N O, 3(C7 H8), C7 H9, H2 O'
_chemical_formula_sum            'C129 H201 Cr7 F8 N O34 Zn'
_chemical_formula_weight         2891.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.7006(4)
_cell_length_b                   30.9417(6)
_cell_length_c                   33.8959(6)
_cell_measurement_reflns_used    45576
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.5060
_cell_measurement_theta_min      2.4690
_cell_volume                     30101.1(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega   85.23  262.73   1.2500   37.3740
omega____ theta____ kappa____ phi______ frames
    -      109.7669   73.8669  -27.8806 142

  2 omega   66.15  248.65   1.2500   37.3740
omega____ theta____ kappa____ phi______ frames
    -       95.6950   73.8669   81.0644 146

  3 phi   -156.66  180.67   1.2494   37.3760
omega____ theta____ kappa____ phi______ frames
 -50.7816  -39.9913   73.8669     -     270

  4 omega   87.55  260.05   1.2500   37.3740
omega____ theta____ kappa____ phi______ frames
    -      112.0919   73.8669    7.8275 138

  5 omega   81.71  264.21   1.2500   37.3740
omega____ theta____ kappa____ phi______ frames
    -      111.2488   73.8669  -56.6825 146

  6 omega -103.92   78.58   1.2500   37.3740
omega____ theta____ kappa____ phi______ frames
    -      -74.3822   73.8669  159.4200 146

  7 omega -108.74   72.51   1.2500   37.3740
omega____ theta____ kappa____ phi______ frames
    -      -79.2000   73.8669 -102.2906 145

  8 phi   -114.38  247.94   1.2494   37.3760
omega____ theta____ kappa____ phi______ frames
 -89.5044  112.2859   73.8669     -     290
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      0.0411491000
_diffrn_orient_matrix_UB_12      0.0316420000
_diffrn_orient_matrix_UB_13      -0.0037622000
_diffrn_orient_matrix_UB_21      0.0083099000
_diffrn_orient_matrix_UB_22      -0.0028627000
_diffrn_orient_matrix_UB_23      0.0448220000
_diffrn_orient_matrix_UB_31      0.0334340000
_diffrn_orient_matrix_UB_32      -0.0383596000
_diffrn_orient_matrix_UB_33      -0.0064584000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            222103
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.366
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             12192
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.895
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1690
_refine_ls_number_reflns         30035
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1338P)^2^+158.5764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2595
_refine_ls_wR_factor_ref         0.2856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21225
_reflns_number_total             30035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09339c2.cif
_cod_data_source_block           xrepw674
_cod_database_code               7122958
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 97.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C18-C17 \\sim C18A-C17 \\sim C19A-C17 \\sim C19-C17 \\sim C20A-C17 \\sim
C20-C17
 with sigma of 0.002
 C37A-C36 \\sim C37-C36 \\sim C39-C37 \\sim C40A-C37A \\sim C40-C37 \\sim
C38A-C37A \\sim C38-C37 ~
 C39A-C37A
 with sigma of 0.002
3. Rigid body (RIGU) restrains
 C18, C19, C20, C17, C19A, C20A, C18A, C16, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C119, C116, C115, C117, C121, C120, C118
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C126, C125, C124, C123, C122, C128, C127
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C38, C39, C37, C40, C38A, C40A, C39A, C37A, C36, O16, O15
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=
 Sof(H40F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C37A)=1-FVAR(2)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C37)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
5.a Free rotating group:
 O35(H35D,H35E)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C92(H92A,H92B), C90(H90A,H90B), C91(H91A,H91B), C120(H12D,H12E)
5.c Me refined with riding coordinates:
 C43(H43A,H43B,H43C), C28(H28A,H28B,H28C), C77(H77A,H77B,H77C), C62(H62A,H62B,
 H62C), C44(H44A,H44B,H44C), C13(H13A,H13B,H13C), C72(H72A,H72B,H72C), C8(H8A,
 H8B,H8C), C78(H78A,H78B,H78C), C38(H38A,H38B,H38C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C3(H3A,H3B,H3C),
  C73(H73A,H73B,H73C), C33(H33A,H33B,H33C), C4(H4A,H4B,H4C), C23(H23A,H23B,
 H23C), C67(H67A,H67B,H67C), C58(H58A,H58B,H58C), C53(H53A,H53B,H53C), C68(H68A,
 H68B,H68C), C34(H34A,H34B,H34C), C59(H59A,H59B,H59C), C54(H54A,H54B,H54C),
 C24(H24A,H24B,H24C), C48(H48A,H48B,H48C), C14(H14A,H14B,H14C), C9(H9A,H9B,H9C),
  C63(H63A,H63B,H63C), C49(H49A,H49B,H49C), C69(H69A,H69B,H69C), C55(H55A,H55B,
 H55C), C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C50(H50A,H50B,H50C), C29(H29A,
 H29B,H29C), C10(H10A,H10B,H10C), C79(H79A,H79B,H79C), C64(H64A,H64B,H64C),
 C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C60(H60A,H60B,
 H60C), C15(H15A,H15B,H15C), C74(H74A,H74B,H74C), C30(H30A,H30B,H30C),
 C107(H10D,H10E,H10F), C114(H11A,H11B,H11C), C121(H12A,H12B,H12C), C128(H12F,
 H12G,H12H), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C18A(H18D,H18E,H18F),
 C38A(H38D,H38E,H38F), C40A(H40D,H40E,H40F), C39A(H39D,H39E,H39F)
5.d Aromatic/amide H refined with riding coordinates:
 C88(H88), C87(H87), C99(H99), C100(H100), C95(H95), C84(H84), C94(H94),
 C96(H96), C82(H82), C81(H81), C98(H98), C85(H85), C97(H97), C102(H102),
 C106(H106), C104(H104), C103(H103), C105(H105), C110(H110), C109(H109),
 C111(H111), C113(H113), C112(H112), C116(H116), C117(H117), C118(H118),
 C119(H119), C123(H123), C124(H124), C127(H127), C126(H126), C125(H125)
5.e Idealised tetrahedral OH refined as rotating group:
 O34(H34)
;
_shelx_res_checksum              55909
_olex2_submission_special_instructions 'No special instructions were received'