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_4120974
_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_sum            'C78 H87 B F15 Mo N5 O6'
_chemical_formula_weight         1582.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.449(2)
_cell_angle_beta                 90.293(2)
_cell_angle_gamma                118.4090(10)
_cell_formula_units_Z            4
_cell_length_a                   19.9236(16)
_cell_length_b                   20.4231(16)
_cell_length_c                   22.4064(17)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      2.19
_cell_volume                     8018.6(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatech I\mS multilayer optics'
_diffrn_radiation_source         'I\mS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42969
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.9273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       needle
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         5.916
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2366
_refine_ls_number_reflns         42969
_refine_ls_number_restraints     5742
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0909
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^2^+21.7131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2651
_refine_ls_wR_factor_ref         0.2834
_reflns_number_gt                29985
_reflns_number_total             42969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408964g_si_001_2.cif
_cod_data_source_block           x12156-sr
_cod_database_code               4120974