Designing new ligands: asymmetric cyclopropanation by Cu(i) complexes based on functionalised pyridine-containing macrocyclic ligands
Caselli, Alessandro; Cesana, Francesca; Gallo, Emma; Casati, Nicola; Macchi, Piero; Sisti, Massimo; Celentano, Giuseppe; Cenini, Sergio; Dalton Transactions  (2008) 4202–4205; doi:10.1039/b809317m

data_7004623
_publ_section_title
;
 Designing new ligands: asymmetric cyclopropanation by Cu(i) complexes
 based on functionalised pyridine-containing macrocyclic ligands
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              4202
_journal_page_last               4205
_journal_paper_doi               10.1039/b809317m
_journal_year                    2008
_chemical_absolute_configuration syn
_chemical_formula_sum            'C41 H47 B Cl2 Cu F4 N5 O4 S2'
_chemical_formula_weight         959.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-04-03T15:42:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 93.652(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   9.758(5)
_cell_length_b                   15.027(5)
_cell_length_c                   15.102(5)
_cell_measurement_reflns_used    364
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      17.39
_cell_measurement_theta_min      3.02
_cell_volume                     2210.0(15)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR97 - A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano,
C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori,
R. Spagna, J. Appl. Cryst. (1999) 32, 115-119.
;
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.1323
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23241
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS - Bruker/Siemens - V2.03'
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8712
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                5179
_reflns_number_total             8712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809317m.txt
_cod_data_source_block           5b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7004623