The rapid synthesis and dynamic behaviour of an isophthalamide [2]catenane.
Marrs, Calum N.; Evans, Nicholas H.; Organic & biomolecular chemistry 13 (2015) 11021–11025; doi:10.1039/c5ob01770j

data_7154718
_publ_section_title
;
 The rapid synthesis and dynamic behaviour of an isophthalamide
 [2]catenane.
;
_journal_issue                   45
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              11021
_journal_page_last               11025
_journal_paper_doi               10.1039/c5ob01770j
_journal_volume                  13
_journal_year                    2015
_chemical_formula_moiety         'C28 H30 N2 O5'
_chemical_formula_sum            'C28 H30 N2 O5'
_chemical_formula_weight         474.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2015-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6388(3)
_cell_length_b                   9.0437(3)
_cell_length_c                   24.8594(8)
_cell_measurement_reflns_used    3389
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      72.9510
_cell_measurement_theta_min      6.0240
_cell_volume                     2391.83(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2299
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1368958000
_diffrn_orient_matrix_UB_12      0.0563675000
_diffrn_orient_matrix_UB_13      -0.0010249000
_diffrn_orient_matrix_UB_21      -0.0214819000
_diffrn_orient_matrix_UB_22      -0.0798366000
_diffrn_orient_matrix_UB_23      -0.0540014000
_diffrn_orient_matrix_UB_31      -0.0423392000
_diffrn_orient_matrix_UB_32      -0.1395727000
_diffrn_orient_matrix_UB_33      0.0302801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5120
_diffrn_reflns_point_group_measured_fraction_full 0.721
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.110
_diffrn_reflns_theta_min         6.051
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
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            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform'
_exptl_crystal_size_max          0.1335
_exptl_crystal_size_mid          0.0844
_exptl_crystal_size_min          0.0826
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.08(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0319P)^2^+0.4787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.398
_reflns_Friedel_fraction_full    0.437
_reflns_Friedel_fraction_max     0.401
_reflns_number_gt                3207
_reflns_number_total             3287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob01770j2.cif
_cod_data_source_block           macrocycle
_cod_depositor_comments
'Adding full bibliography for 7154718--7154719.cif.'
_cod_database_code               7154718
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H30 N2 O5'
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C5(H5A,H5B), C12(H12A,H12B), C15(H15A,H15B),
 C26(H26A,H26B), C22(H22A,H22B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C33(H33), C17(H17), C31(H31), C21(H21), C32(H32),
 C14(H14), C18(H18), C20(H20), C13(H13), C35(H35)
;
_shelx_res_checksum              97937
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'