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_4120973
_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         'C66 H63 B F15 Mo N5 O6, 3(C7 H8)'
_chemical_formula_sum            'C87 H87 B F15 Mo N5 O6'
_chemical_formula_weight         1690.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                112.253(2)
_cell_angle_beta                 105.282(2)
_cell_angle_gamma                105.710(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1951(15)
_cell_length_b                   14.829(2)
_cell_length_c                   14.876(2)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.22
_cell_measurement_theta_min      2.64
_cell_volume                     2005.9(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            107499
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.9734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.976
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         22751
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+1.5936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                20941
_reflns_number_total             22751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408964g_si_001_1.cif
_cod_data_source_block           x12155
_cod_database_code               4120973