Macrocyclic <i>vs.</i> [2]catenane btp structures: influence of (aryl) substitution on the self templation of btp ligands in macrocyclic synthesis.
McCarney, Eoin P.; McCarthy, William J.; Lovitt, June I.; Gunnlaugsson, Thorfinnur; Organic & biomolecular chemistry 19 (2021) 10189–10200; doi:10.1039/d1ob02032c

data_7158404
_publ_section_title
;
 Macrocyclic <i>vs.</i> [2]catenane btp structures: influence of (aryl)
 substitution on the self templation of btp ligands in macrocyclic
 synthesis.
;
_journal_issue                   46
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              10189
_journal_page_last               10200
_journal_paper_doi               10.1039/d1ob02032c
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C29 H43 N7'
_chemical_formula_sum            'C29 H43 N7'
_chemical_formula_weight         489.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-14 deposited with the CCDC.	2021-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.78(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.58(2)
_cell_length_b                   16.258(19)
_cell_length_c                   10.196(11)
_cell_measurement_reflns_used    101
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      54.082
_cell_measurement_theta_min      35.708
_cell_volume                     2853(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 Kappa Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       APEX2
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3981
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        60.189
_diffrn_reflns_theta_max         60.189
_diffrn_reflns_theta_min         2.567
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.65
_diffrn_source_power             0.0290745
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           44.73
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.8038.
The \l/2 correction factor is Not present.
;
_exptl.absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for 
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     931
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0904
_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^)+(0.1357P)^2^+1.8089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.3128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1985
_reflns_number_total             3981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob02032c2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7158403--7158405.cif.'
_cod_database_code               7158404
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1. Shared sites
{H30C, H30A}
2. Others
 Fixed Uiso: H3(0.154) H4(0.164) H5(0.148) H11(0.122) H12A(0.155) H12B(0.155)
 H13C(0.158) H13D(0.158) H13A(0.158) H13B(0.158) H14A(0.179) H14B(0.179)
 H15A(0.171) H15B(0.171) H16A(0.147) H16B(0.147) H17A(0.195) H17B(0.195)
 H18A(0.212) H18B(0.212) H19A(0.211) H19B(0.211) H20A(0.232) H20B(0.232)
 H23A(0.238) H23B(0.238) H24A(0.194) H24B(0.194) H25A(0.175) H25B(0.175)
 H26A(0.141) H26B(0.141) H27A(0.153) H27B(0.153) H28A(0.129) H28B(0.129)
 H29A(0.191) H29B(0.191) H30C(0.198) H30D(0.198) H30A(0.198) H30B(0.198)
 H31A(0.184) H31B(0.184) H36(0.132) H37A(0.122) H37B(0.122) H38A(0.147)
 H38B(0.147) H39A(0.176) H39B(0.176) H40A(0.161) H40B(0.161) H41A(0.178)
 H41B(0.178) H42A(0.169) H42B(0.169) H43A(0.172) H43B(0.172) H44A(0.275)
 H44(0.275) H45A(0.278) H45(0.278) H46A(0.247) H46B(0.247) H47A(0.226)
 H47B(0.226) H48A(0.22) H48B(0.22) H49A(0.182) H49B(0.182) H50A(0.157)
 H50B(0.157) H51A(0.159) H51B(0.159) H52A(0.137) H52B(0.137)
 Fixed X: H3(0.637985) H4(0.729171) H5(0.777007) H11(0.680034) H12A(0.736595)
 H12B(0.707186) H13C(0.863745) H13D(0.817506) H13A(0.866518) H13B(0.820563)
 H14A(0.854065) H14B(0.792545) H15A(0.887588) H15B(0.95159) H16A(0.88318)
 H16B(0.952392) H17A(1.035472) H17B(0.966233) H18A(1.056924) H18B(1.028074)
 H19A(0.917334) H19B(0.909032) H20A(1.02058) H20B(0.957372) H23A(0.815301)
 H23B(0.850676) H24A(0.775191) H24B(0.724037) H25A(0.753156) H25B(0.675538)
 H26A(0.642176) H26B(0.719304) H27A(0.672759) H27B(0.598671) H28A(0.630446)
 H28B(0.557338) H29A(0.510097) H29B(0.577175) H30C(0.440708) H30D(0.51024)
 H30A(0.439077) H30B(0.50706) H31A(0.393783) H31B(0.426389) H36(0.548438)
 H37A(0.815437) H37B(0.871843) H38A(0.907704) H38B(0.962024) H39A(1.0155)
 H39B(0.981948) H40A(0.90148) H40B(0.875883) H41A(1.011235) H41B(1.00277)
 H42A(0.889004) H42B(0.889006) H43A(1.009434) H43B(1.003354) H44A(0.895256)
 H44(0.905969) H45A(0.91329) H45(0.915188) H46A(0.872286) H46B(0.815179)
 H47A(0.801745) H47B(0.73869) H48A(0.773377) H48B(0.714095) H49A(0.694674)
 H49B(0.635444) H50A(0.667624) H50B(0.606498) H51A(0.592893) H51B(0.528498)
 H52A(0.575974) H52B(0.50696)
 Fixed Y: H3(0.043072) H4(-0.048835) H5(-0.035895) H11(0.183524)
 H12A(0.127491) H12B(0.20829) H13C(0.16548) H13D(0.240218) H13A(0.167241)
 H13B(0.236993) H14A(0.237866) H14B(0.299671) H15A(0.373163) H15B(0.306492)
 H16A(0.413252) H16B(0.350227) H17A(0.425923) H17B(0.488107) H18A(0.5409)
 H18B(0.470824) H19A(0.579363) H19B(0.527139) H20A(0.635495) H20B(0.686951)
 H23A(0.711618) H23B(0.802281) H24A(0.815064) H24B(0.813718) H25A(0.668868)
 H25B(0.722173) H26A(0.692807) H26B(0.638369) H27A(0.543611) H27B(0.60029)
 H28A(0.527054) H28B(0.582731) H29A(0.470394) H29B(0.418285) H30C(0.462977)
 H30D(0.411179) H30A(0.461195) H30B(0.409786) H31A(0.33797) H31B(0.347102)
 H36(0.24784) H37A(0.305762) H37B(0.234034) H38A(0.347489) H38B(0.270333)
 H39A(0.383399) H39B(0.324467) H40A(0.467821) H40B(0.411503) H41A(0.514328)
 H41B(0.44507) H42A(0.571115) H42B(0.506411) H43A(0.566022) H43B(0.634107)
 H44A(0.619317) H44(0.609219) H45A(0.746379) H45(0.75453) H46A(0.807758)
 H46B(0.815734) H47A(0.704431) H47B(0.770121) H48A(0.619092) H48B(0.686562)
 H49A(0.60493) H49B(0.672464) H50A(0.518405) H50B(0.585517) H51A(0.511703)
 H51B(0.569007) H52A(0.410952) H52B(0.467222)
 Fixed Z: H3(0.104383) H4(0.215633) H5(0.450073) H11(0.663017) H12A(1.004838)
 H12B(0.919825) H13C(1.026125) H13D(1.074497) H13A(1.015242) H13B(1.079075)
 H14A(0.817448) H14B(0.857167) H15A(0.992887) H15B(0.97899) H16A(0.766913)
 H16B(0.762183) H17A(0.930801) H17B(0.939623) H18A(0.811188) H18B(0.701907)
 H19A(0.773062) H19B(0.638668) H20A(0.624286) H20B(0.68236) H23A(0.316353)
 H23B(0.34364) H24A(0.520079) H24B(0.370604) H25A(0.533674) H25B(0.522183)
 H26A(0.288659) H26B(0.301705) H27A(0.439318) H27B(0.442706) H28A(0.209143)
 H28B(0.212744) H29A(0.322456) H29B(0.282583) H30C(0.107516) H30D(0.068591)
 H30A(0.106901) H30B(0.064806) H31A(0.092959) H31B(0.25089) H36(0.353887)
 H37A(0.860789) H37B(0.829003) H38A(1.04895) H38B(1.034433) H39A(0.950641)
 H39B(0.827127) H40A(0.887626) H40B(0.75674) H41A(0.817029) H41B(0.702541)
 H42A(0.702489) H42B(0.58377) H43A(0.548236) H43B(0.660242) H44A(0.406171)
 H44(0.415029) H45A(0.580935) H45(0.571613) H46A(0.347601) H46B(0.450435)
 H47A(0.232099) H47B(0.25724) H48A(0.403339) H48B(0.439359) H49A(0.184518)
 H49B(0.220379) H50A(0.360179) H50B(0.391531) H51A(0.131432) H51B(0.177408)
 H52A(0.301342) H52B(0.33632)
;
_shelx_res_checksum              82945
_olex2_submission_special_instructions 'No special instructions were received'