Isolation of (CO)1- and (CO2)1-Radical Complexes of Rare Earths via Ln(NR2)3/K Reduction and [K2(18-crown-6)2]2+ Oligomerization
Ming Fang; Joy H. Farnaby; Joseph W. Ziller; Jefferson E. Bates; Filipp Furche; William J. Evans; Journal of the American Chemical Society 134 (2012) 6064–6067; doi:10.1021/ja211220r

data_4117780
_publ_section_title
;
 Isolation of (CO)1- and (CO2)1-Radical Complexes of Rare Earths via
 Ln(NR2)3/K Reduction and [K2(18-crown-6)2]2+ Oligomerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6064
_journal_page_last               6067
_journal_paper_doi               10.1021/ja211220r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C78 H196 K2 Lu2 N6 O18 Si12'
_chemical_formula_weight         2271.63
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXTL
_cell_angle_alpha                61.9215(9)
_cell_angle_beta                 66.3760(10)
_cell_angle_gamma                65.6289(10)
_cell_formula_units_Z            1
_cell_length_a                   15.3990(14)
_cell_length_b                   15.6526(14)
_cell_length_c                   15.8991(15)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.38
_cell_volume                     2976.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33933
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  0.6573
_exptl_absorpt_correction_T_min  0.5379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.936
_refine_diff_density_min         -2.145
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         12996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0312P)^2^+7.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                11788
_reflns_number_total             12996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211220r_si_010.cif
_cod_data_source_block           jhf7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4117780