Discrete, Solvent-Free Alkaline-Earth Metal Cations: Metal...Fluorine Interactions and ROP Catalytic Activity
Yann Sarazin; Bo Liu; Thierry Roisnel; Laurent Maron; Jean-François Carpentier; Journal of the American Chemical Society 133 (2011) 9069–9087; doi:10.1021/ja2024977

data_4106257
_publ_section_title
;
 Discrete, Solvent-Free Alkaline-Earth Metal Cations: Metal...Fluorine
 Interactions and ROP Catalytic Activity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9069
_journal_page_last               9087
_journal_paper_doi               10.1021/ja2024977
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'2(C28 H44 Ca2 F12 N2 O10), 4(C36 H2 B2 F30 N), 3(C H2 Cl2)'
_chemical_formula_sum            'C203 H102 B8 Ca4 Cl6 F144 N8 O20'
_chemical_formula_weight         6168.43
_chemical_name_systematic
;
 ?
;
_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_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             2010-09-13T19:32:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                76.723(2)
_cell_angle_beta                 86.104(2)
_cell_angle_gamma                63.110(2)
_cell_formula_units_Z            2
_cell_length_a                   17.2351(8)
_cell_length_b                   18.9583(8)
_cell_length_c                   40.8891(17)
_cell_measurement_reflns_used    7062
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.54
_cell_measurement_theta_min      2.22
_cell_measurement_wavelength     0.71073
_cell_volume                     11587.4(9)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SAINT (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999))'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.1445
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            114608
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       prism
_exptl_crystal_F_000             6108
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.488
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0051(2)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3509
_refine_ls_number_reflns         51686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2617
_reflns_number_gt                25558
_reflns_number_total             51686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2024977_si_001_7.cif
_cod_data_source_block           15
_cod_database_code               4106257