[3]rotaxanes composed of two dibenzo-24-crown-8 ether wheels and an azamacrocyclic complex.
Woźny, Mateusz; Więckowska, Agnieszka; Trzybiński, Damian; Sutuła, Szymon; Domagała, Sławomir; Woźniak, Krzysztof; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15845–15856; doi:10.1039/c8dt03225d

data_7047889
_publ_section_title
;
 [3]rotaxanes composed of two dibenzo-24-crown-8 ether wheels and an
 azamacrocyclic complex.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15845
_journal_page_last               15856
_journal_paper_doi               10.1039/c8dt03225d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C34 H40 N12 Ni O12, 2(C24 H32 O8), 2(F6 P), 0.89(C H4 O), 1.68(C3 H6 O), 0.32(H2 O)'
_chemical_formula_sum            'C87.92 H118.26 F12 N12 Ni O30.89 P2'
_chemical_formula_weight         2186.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-07-16 deposited with the CCDC.
2018-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                76.0271(19)
_cell_angle_beta                 89.369(2)
_cell_angle_gamma                81.8124(19)
_cell_formula_units_Z            1
_cell_length_a                   11.7523(3)
_cell_length_b                   13.4144(3)
_cell_length_c                   16.3890(4)
_cell_measurement_reflns_used    19878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2850
_cell_measurement_theta_min      2.7690
_cell_volume                     2480.98(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -42.00   92.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 134

  2 omega -101.00  -35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000    0.0000 66

  3 omega -103.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.5000   61.0000   90.0000 135

  4 omega -156.00  -80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.5000  -94.0000   30.0000 76

  5 omega  -48.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.5000   30.0000  -90.0000 79

  6 omega  -48.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.5000   30.0000   60.0000 79

  7 omega   94.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000  125.0000  -30.0000 58

  8 omega   94.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000  125.0000   90.0000 58

  9 omega   23.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000 -125.0000 -180.0000 98

 10 omega   16.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000   81.0000  121.4992 30

 11 omega   18.00  153.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000   61.0000  -60.0000 135

 12 omega   16.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000   81.0000   54.3270 30

 13 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000 -180.0000 86

 14 omega   21.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -77.0000  -60.0000 144

 15 omega   21.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000    0.0000  -30.0000 157

 16 omega   28.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -25.0000  120.0000 66

 17 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000  -90.0000 86

 18 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000  120.0000 86

 19 omega   30.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -37.0000  -30.0000 62

 20 omega   21.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -77.0000 -120.0000 144

 21 omega   21.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -77.0000   60.0000 144

 22 omega   28.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -25.0000 -120.0000 66

 23 omega   42.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000   25.0000   60.0000 136

 24 omega   21.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -77.0000  150.0000 144

 25 omega   30.00  104.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -50.0000  150.0000 74

 26 omega  100.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  111.0000 -120.0000 78

 27 omega   57.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  178.0000  120.0000 93

 28 omega   30.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -37.0000 -150.0000 62

 29 omega   24.00  169.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -91.0000 -120.0000 145

 30 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000 -120.0000 86

 31 omega   25.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -12.0000    0.0000 153

 32 omega   30.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -37.0000  150.0000 62

 33 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000   60.0000 86

 34 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000  -30.0000 86

 35 omega   28.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -25.0000 -150.0000 66

 36 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000    0.0000 86

 37 omega   77.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000   63.0000 -180.0000 101

 38 omega   79.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000   50.0000    0.0000 99

 39 omega   30.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -37.0000   60.0000 62

 40 omega   27.00  165.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -63.0000 -120.0000 138

 41 omega   29.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000 -111.0000   90.0000 86

 42 omega   57.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  178.0000   30.0000 93

 43 omega  100.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  111.0000  -60.0000 78

 44 omega   74.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000   37.0000 -120.0000 104

 45 omega   57.00  150.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  178.0000 -120.0000 93

 46 omega   42.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000   25.0000   60.0000 136

 47 omega   24.00  169.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -91.0000  -30.0000 145

 48 omega   24.00  169.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -91.0000   60.0000 145

 49 omega   30.00  103.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      121.0000  -49.0000  109.0865 73

 50 omega  -92.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 134

 51 omega  -44.00  100.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -180.0000 144

 52 omega  -92.00   42.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 134

 53 omega -152.00  -58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -60.5000  -45.0000  150.0000 94

 54 omega   16.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000   82.0000  -11.1418 29

 55 omega   16.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       60.5000   81.0000  179.2560 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1309840000
_diffrn_orient_matrix_UB_12      -0.0045453000
_diffrn_orient_matrix_UB_13      0.0098356000
_diffrn_orient_matrix_UB_21      0.0115216000
_diffrn_orient_matrix_UB_22      -0.1177429000
_diffrn_orient_matrix_UB_23      0.0388021000
_diffrn_orient_matrix_UB_31      0.0161270000
_diffrn_orient_matrix_UB_32      -0.0204524000
_diffrn_orient_matrix_UB_33      -0.0882399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51296
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.809
_diffrn_reflns_theta_min         2.779
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       plate
_exptl_crystal_F_000             1143
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         10402
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0625P)^2^+1.0292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9022
_reflns_number_total             10402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03225d2.cif
_cod_data_source_block           dinitro_benz_3rot
_cod_depositor_comments
'Adding full bibliography for 7047888--7047889.cif.'
_cod_database_code               7047889
_chemical_oxdiff_formula         'C60 H90 Ni1 O16 N12'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.027) H4(0.039) H1A(0.028) H1B(0.028) H2(0.024) H4A(0.025)
 H5A(0.028) H5B(0.028) H6(0.025) H7A(0.03) H7B(0.03) H8A(0.029) H8B(0.029)
 H9A(0.033) H9B(0.033) H10A(0.035) H10B(0.035) H13(0.037) H15(0.046) H17(0.044)
 H19(0.035) H20(0.039) H21(0.037) H22(0.033) H24A(0.033) H24B(0.033)
 H25A(0.031) H25B(0.031) H26A(0.03) H26B(0.03) H27A(0.03) H27B(0.03)
 H28A(0.034) H28B(0.034) H29A(0.032) H29B(0.032) H31(0.042) H32(0.051)
 H33(0.058) H34(0.051) H36A(0.047) H36B(0.047) H37A(0.05) H37B(0.05)
 H38A(0.049) H38B(0.049) H39A(0.046) H39B(0.046) H40A(0.039) H40B(0.039)
 H41A(0.035) H41B(0.035) H16(0.209) H45A(0.061) H45B(0.061) H45C(0.061)
 H43A(0.09) H43B(0.09) H43C(0.09) H44A(0.065) H44B(0.065) H44C(0.065)
 H17A(0.101) H17B(0.101)
 Fixed X: Ni1(0) H3(0.2788) H4(0.2598) H1A(0.1977) H1B(0.2167) H2(0.2342)
 H4A(0.0744) H5A(-0.0106) H5B(-0.0741) H6(0.1908) H7A(0.3117) H7B(0.3998)
 H8A(0.2814) H8B(0.1735) H9A(0.3751) H9B(0.2727) H10A(0.1454) H10B(0.2593)
 H13(0.072) H15(0.0139) H17(0.2213) H19(-0.2076) H20(-0.2848) H21(-0.2112) H22(-
 0.057) H24A(0.1133) H24B(0.0349) H25A(0.1845) H25B(0.22) H26A(0.3079)
 H26B(0.3742) H27A(0.5167) H27B(0.5083) H28A(0.5817) H28B(0.5892) H29A(0.4558)
 H29B(0.575) H31(0.5393) H32(0.5593) H33(0.4873) H34(0.3964) H36A(0.2785)
 H36B(0.4145) H37A(0.3938) H37B(0.355) H38A(0.2121) H38B(0.2639) H39A(0.0672)
 H39B(0.0306) H40A(-0.0726) H40B(-0.0217) H41A(-0.1709) H41B(-0.0808)
 H16(0.5283) H45A(0.6533) H45B(0.6161) H45C(0.5381) H43A(0.4027) H43B(0.3927)
 H43C(0.2818) H44A(0.2514) H44B(0.3888) H44C(0.3272) H17A(0.4573) H17B(0.36)
 Fixed Y: Ni1(1) H3(0.6304) H4(0.064) H1A(0.8842) H1B(0.9943) H2(0.7858)
 H4A(0.832) H5A(1.0564) H5B(0.958) H6(0.682) H7A(0.5316) H7B(0.5095)
 H8A(0.4117) H8B(0.4532) H9A(0.3184) H9B(0.3641) H10A(0.2751) H10B(0.2167) H13(-
 0.0654) H15(-0.2636) H17(-0.0437) H19(0.769) H20(0.8939) H21(0.8909)
 H22(0.7643) H24A(0.6739) H24B(0.5843) H25A(0.4639) H25B(0.5059) H26A(0.6903)
 H26B(0.586) H27A(0.5764) H27B(0.6862) H28A(0.7576) H28B(0.6414) H29A(0.7056)
 H29B(0.7516) H31(1.0168) H32(1.1379) H33(1.1144) H34(0.9707) H36A(0.8346)
 H36B(0.8075) H37A(0.6371) H37B(0.6571) H38A(0.56) H38B(0.5069) H39A(0.4817)
 H39B(0.6024) H40A(0.4862) H40B(0.4489) H41A(0.5992) H41B(0.6645) H16(0.0532)
 H45A(0.1837) H45B(0.0996) H45C(0.2103) H43A(0.2645) H43B(0.3351) H43C(0.33)
 H44A(0.2584) H44B(0.248) H44C(0.1468) H17A(0.1268) H17B(0.1668)
 Fixed Z: Ni1(0) H3(0.0778) H4(0.4636) H1A(-0.1336) H1B(-0.1173) H2(-0.0011)
 H4A(0.2113) H5A(0.1792) H5B(0.2197) H6(0.2171) H7A(0.2477) H7B(0.1769)
 H8A(0.1289) H8B(0.1786) H9A(0.2578) H9B(0.3096) H10A(0.244) H10B(0.211)
 H13(0.3747) H15(0.5975) H17(0.5914) H19(0.1467) H20(0.0269) H21(-0.105) H22(-
 0.1187) H24A(-0.1081) H24B(-0.1052) H25A(-0.0178) H25B(-0.1131) H26A(-0.1227)
 H26B(-0.1429) H27A(-0.0395) H27B(-0.107) H28A(0.0057) H28B(0.0628) H29A(0.157)
 H29B(0.1534) H31(0.0554) H32(0.1336) H33(0.2688) H34(0.3264) H36A(0.3577)
 H36B(0.3758) H37A(0.349) H37B(0.4384) H38A(0.4714) H38B(0.3986) H39A(0.4359)
 H39B(0.3921) H40A(0.3391) H40B(0.2587) H41A(0.2255) H41B(0.2544) H16(0.4536)
 H45A(0.4555) H45B(0.5344) H45C(0.5037) H43A(0.4739) H43B(0.5403) H43C(0.4865)
 H44A(0.6777) H44B(0.6792) H44C(0.71) H17A(0.4937) H17B(0.5343)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'