Trivalent [(C5Me5)2(THF)Ln]2(μ-η2:η2-N2) Complexes as Reducing Agents Including the Reductive Homologation of CO to a Ketene Carboxylate, (μ-η4-O2CCCO)2-
William J. Evans; David S. Lee; Joseph W. Ziller; Nikolas Kaltsoyannis; Journal of the American Chemical Society 128 (2006) 14176–14184; doi:10.1021/ja0640851

data_4111036
_publ_section_title
;
 Trivalent [(C5Me5)2(THF)Ln]2(\m-\h2:\h2-N2) Complexes as Reducing Agents
 Including the Reductive Homologation of CO to a Ketene Carboxylate,
 (\m-\h4-O2CCCO)2-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14176
_journal_page_last               14184
_journal_paper_doi               10.1021/ja0640851
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C118 H160 La4 O8'
_chemical_formula_weight         2262.10
_chemical_name_systematic
; 
 ? 
;
_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                91.539(7)
_cell_angle_beta                 114.067(7)
_cell_angle_gamma                109.738(7)
_cell_formula_units_Z            1
_cell_length_a                   14.234(6)
_cell_length_b                   14.365(6)
_cell_length_c                   15.917(7)
_cell_measurement_temperature    163(2)
_cell_volume                     2745(2)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26378
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.8093
_exptl_absorpt_correction_T_min  0.6322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.217
_refine_diff_density_min         -2.152
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+6.4073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                6679
_reflns_number_total             9359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0640851si20060609_054913.cif
_cod_data_source_block           dl41
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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_original_formula_sum        'C94 H136 La4 O8 4(C6H6)'
_cod_database_code               4111036