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_4117779
_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 H190 K2 Lu2 N6 O21 Si12'
_chemical_formula_weight         2313.58
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0088(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.4359(10)
_cell_length_b                   18.7392(8)
_cell_length_c                   25.6999(10)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.26
_cell_volume                     11935.4(8)
_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      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            67902
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  0.8104
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         13174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+14.3355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                10409
_reflns_number_total             13174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211220r_si_009.cif
_cod_data_source_block           jhf6
_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 
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_cod_database_code               4117779