Asymmetric cyclopropanation of olefins catalysed by Cu(i) complexes of chiral pyridine-containing macrocyclic ligands (Pc-L*).
Castano, Brunilde; Guidone, Stefano; Gallo, Emma; Ragaini, Fabio; Casati, Nicola; Macchi, Piero; Sisti, Massimo; Caselli, Alessandro; Dalton transactions (Cambridge, England : 2003) 42 (2013) 2451–2462; doi:10.1039/c2dt32347h

data_7020893
_publ_section_title
;
 Asymmetric cyclopropanation of olefins catalysed by Cu(i) complexes of
 chiral pyridine-containing macrocyclic ligands (Pc-L*).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2451
_journal_page_last               2462
_journal_paper_doi               10.1039/c2dt32347h
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C39 H44 N4 O4 S2'
_chemical_formula_weight         696.9
_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_date             2012-09-27T13:26:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7670(4)
_cell_length_b                   14.2550(5)
_cell_length_c                   25.9891(15)
_cell_measurement_reflns_used    1674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2949
_cell_measurement_theta_min      2.8521
_cell_volume                     3618.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0022231
_diffrn_orient_matrix_UB_12      -0.0496953
_diffrn_orient_matrix_UB_13      0.0011153
_diffrn_orient_matrix_UB_21      0.0358123
_diffrn_orient_matrix_UB_22      -0.0024968
_diffrn_orient_matrix_UB_23      -0.0237048
_diffrn_orient_matrix_UB_31      0.0631448
_diffrn_orient_matrix_UB_32      -0.0003094
_diffrn_orient_matrix_UB_33      0.0134748
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11009
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  1.172
_exptl_absorpt_correction_T_min  1.071
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.1736
_exptl_crystal_size_mid          0.0842
_exptl_crystal_size_min          0.0834
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.09
_reflns_number_gt                3421
_reflns_number_total             6595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32347h.txt
_cod_data_source_block           4d
_cod_database_code               7020893