Dinitrogen Reduction via Photochemical Activation of Heteroleptic Tris(cyclopentadienyl) Rare-Earth Complexes
Megan E. Fieser; Jefferson E. Bates; Joseph W. Ziller; Filipp Furche; William J. Evans; Journal of the American Chemical Society 135 (2013) 3804–3807; doi:10.1021/ja400664s

data_4119473
_publ_section_title
;
 Dinitrogen Reduction via Photochemical Activation of Heteroleptic
 Tris(cyclopentadienyl) Rare-Earth Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3804
_journal_page_last               3807
_journal_paper_doi               10.1021/ja400664s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C29 H43 Dy'
_chemical_formula_weight         554.13
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                92.3266(5)
_cell_angle_beta                 90.3471(5)
_cell_angle_gamma                99.9098(5)
_cell_formula_units_Z            4
_cell_length_a                   10.0370(5)
_cell_length_b                   14.3561(7)
_cell_length_c                   17.7392(8)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.30
_cell_volume                     2515.6(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.904
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30167
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  0.6500
_exptl_absorpt_correction_T_min  0.4468
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         11992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0268P)^2^+0.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                10540
_reflns_number_total             11992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400664s_si_002.cif
_cod_data_source_block           mef4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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               4119473