[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_7047888
_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
'2(C24 H32 O8), C34 H40 N12 Ni O12, 2(C2 H3 N), 2(Cl)'
_chemical_formula_sum            'C86 H110 Cl2 N14 Ni O28'
_chemical_formula_weight         1917.48
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-11
_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                90
_cell_angle_beta                 110.074(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7551(3)
_cell_length_b                   22.9462(4)
_cell_length_c                   16.8432(4)
_cell_measurement_reflns_used    18811
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.6810
_cell_measurement_theta_min      1.9490
_cell_volume                     4630.21(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0266
_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       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33438
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         1.745
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       prism
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0227P)^2^+2.9694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7018
_reflns_number_total             8265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03225d2.cif
_cod_data_source_block           2016_11_03_ss_daszk2-mo_n
_cod_depositor_comments
'Adding full bibliography for 7047888--7047889.cif.'
_cod_original_cell_volume        4630.20(17)
_cod_database_code               7047888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C40(H40A,H40B), C39(H39A,H39B), C38(H38A,H38B), C37(H37A,
 H37B), C36(H36A,H36B), C29(H29A,H29B), C28(H28A,H28B), C27(H27A,H27B),
 C26(H26A,H26B), C25(H25A,H25B), C24(H24A,H24B), C5(H5A,H5B), C1(H1A,H1B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C20(H20), C19(H19), C34(H34), C33(H33), C32(H32),
 C31(H31), C2(H2), C4(H4), C6(H6), C13(H13), C15(H15), C17(H17)
2.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'