Synthesis of Macrocyclic β-Strand Templates by Ring Closing Metathesis
Andrew D. Abell; Nathan A. Alexander; Steven G. Aitken; Hongyuan Chen; James M. Coxon; Matthew A. Jones; Stephen B. McNabb; Andrew Muscroft-Taylor; Journal of Organic Chemistry 74 (2009) 4354–4356; doi:10.1021/jo802723w

data_4024555
_publ_section_title
;
Synthesis of Macrocyclic \b-Strand Templates by Ring Closing Metathesis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4354
_journal_page_last               4356
_journal_paper_doi               10.1021/jo802723w
_journal_volume                  74
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C27 H39 N3 O7'
_chemical_formula_sum            'C27 H39 N3 O7'
_chemical_formula_weight         517.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5967(17)
_cell_length_b                   13.576(3)
_cell_length_c                   22.201(6)
_cell_measurement_reflns_used    7283
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      32.619
_cell_measurement_theta_min      2.310
_cell_volume                     2892.5(11)
_computing_cell_refinement       'APEXII V1.0-27'
_computing_data_collection       'APEXII V1.0-27 (Bruker 2004)'
_computing_data_reduction        'APEXII V1.0-27'
_computing_molecular_graphics
;
Ortep-3 for windows, V1.08 (Farrugia, 1997). Mercury, V1.4, (Bruno et al., 2002)
;
_computing_publication_material  'enCIFER, V1.1 (Allen et al., 2004)'
_computing_structure_refinement  'APEXII V1.0-27'
_computing_structure_solution    'APEXII V1.0-27'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37305
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEXII V1.0-27  (Bruker, 2004) '
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.200
_refine_ls_abs_structure_details 'Friedel pairs were merged'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_coef       0.0216(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         2923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.5007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                2613
_reflns_number_total             2923
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo802723w_si_002.cif
_cod_data_source_block           amtc
_cod_database_code               4024555