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_4119474
_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            'C28 H41 Lu'
_chemical_formula_weight         552.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 114.6008(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.970(2)
_cell_length_b                   10.2044(9)
_cell_length_c                   23.173(2)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.22
_cell_volume                     4938.6(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51639
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    4.009
_exptl_absorpt_correction_T_max  0.6995
_exptl_absorpt_correction_T_min  0.5148
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.390
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         10128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0219P)^2^+33.6713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                8738
_reflns_number_total             10128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400664s_si_003.cif
_cod_data_source_block           mef7
_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_original_cell_volume        4938.8(7)
_cod_database_code               4119474