Self-templated synthesis of amide catenanes and formation of a catenane coordination polymer.
Lewis, James E. M.; Organic & biomolecular chemistry 17 (2019) 2442–2447; doi:10.1039/c9ob00107g

data_7156669
_publ_section_title
;
 Self-templated synthesis of amide catenanes and formation of a catenane
 coordination polymer.
;
_journal_issue                   9
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2442
_journal_page_last               2447
_journal_paper_doi               10.1039/c9ob00107g
_journal_volume                  17
_journal_year                    2019
_chemical_formula_moiety         '2(C29 H33 N3 O7), 6.25(H2 O)'
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_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
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-02-01 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.033(3)
_cell_angle_beta                 100.915(4)
_cell_angle_gamma                105.148(4)
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_cell_measurement_reflns_used    4722
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5960
_cell_measurement_theta_min      2.7810
_cell_volume                     3027.4(2)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.800
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.986
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         2.570
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.099
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_exptl_absorpt_correction_T_min  0.953
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_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.46 (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            Colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1261
_exptl_crystal_size_max          0.637
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_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.208
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_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         11912
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.8550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8665
_reflns_number_total             11912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00107g2.cif
_cod_data_source_block           4g
_cod_depositor_comments
'Adding full bibliography for 7156668--7156670.cif.'
_cod_original_formula_sum        'C58 H78.50 N6 O20.25'
_cod_database_code               7156669
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              79943