Synthesis of a TREN in Which the Aryl Substituents are Part of a 45 Atom Macrocycle
Matthew F. Cain; William P. Forrest; Dmitry V. Peryshkov; Richard R. Schrock; Peter Müller; Journal of the American Chemical Society 135 (2013) 15338–15341; doi:10.1021/ja408964g

data_4120975
_publ_section_title
;
 Synthesis of a TREN in Which the Aryl Substituents are Part of a 45 Atom
 Macrocycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15338
_journal_page_last               15341
_journal_paper_doi               10.1021/ja408964g
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C54 H78 N4 O6, 0.5(C6 H6)'
_chemical_formula_sum            'C57 H81 N4 O6'
_chemical_formula_weight         918.25
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 103.5620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2832(4)
_cell_length_b                   13.3747(3)
_cell_length_c                   20.5415(4)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.62
_cell_measurement_theta_min      3.98
_cell_volume                     5150.08(19)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.878
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67124
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.363
_diffrn_reflns_theta_min         2.830
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       plate
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         8181
_refine_ls_number_restraints     2429
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0653
_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^)+(0.1038P)^2^+3.1052P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5217
_reflns_number_total             8181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja408964g_si_001_3.cif
_cod_data_source_block           x13091
_cod_database_code               4120975
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2012-9
_shelx_res_checksum              35374