Crossing the threshold from accelerated substitution to elimination with a bifunctional macrocycle
Gassensmith, Jeremiah J.; Lee, Jung-Jae; Noll, Bruce C.; Smith, Bradley D.; New Journal of Chemistry 32 (2008) 843–; doi:10.1039/b719658j

data_7051902
_publ_section_title
;
 Crossing the threshold from accelerated substitution to elimination
 with a bifunctional macrocycle
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              843
_journal_paper_doi               10.1039/b719658j
_journal_volume                  32
_journal_year                    2008
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C27 H30 N3 O4 +, Cl -'
_chemical_formula_sum            'C27 H30 Cl N3 O4'
_chemical_formula_weight         495.99
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                99.027(1)
_cell_angle_beta                 104.128(1)
_cell_angle_gamma                102.882(1)
_cell_formula_units_Z            4
_cell_length_a                   11.0581(3)
_cell_length_b                   13.2036(3)
_cell_length_c                   18.3085(5)
_cell_measurement_reflns_used    9338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.38
_cell_measurement_theta_min      2.35
_cell_volume                     2463.12(11)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65637
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.18
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.9211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         16272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0614P)^2^+3.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                13611
_reflns_number_total             16272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719658j.txt
_cod_data_source_block           bcn116noh
_cod_database_code               7051902