(C5Me4H)1−-based reduction of dinitrogen by the mixed ligand tris(polyalkylcyclopentadienyl) lutetium and yttrium complexes, (C5Me5)3−x(C5Me4H)xLn
Mueller, Thomas J.; Fieser, Megan E.; Ziller, Joseph W.; Evans, William J.; Chemical Science 2 (2011) 1992–; doi:10.1039/c1sc00139f

data_1515496
_publ_section_title
;
 (C5Me4H)1&#x2212;-based reduction of dinitrogen by the mixed ligand
 tris(polyalkylcyclopentadienyl) lutetium and yttrium complexes,
 (C5Me5)3&#x2212;x(C5Me4H)xLn
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              1992
_journal_paper_doi               10.1039/c1sc00139f
_journal_volume                  2
_journal_year                    2011
_chemical_formula_sum            'C40 H60 N2 Y2'
_chemical_formula_weight         746.72
_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                77.9317(13)
_cell_angle_beta                 77.8776(13)
_cell_angle_gamma                83.5536(13)
_cell_formula_units_Z            2
_cell_length_a                   10.6716(11)
_cell_length_b                   10.9978(11)
_cell_length_c                   16.7386(17)
_cell_measurement_reflns_used    6454
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.48
_cell_volume                     1873.4(3)
_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      93(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8205
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  0.5837
_exptl_absorpt_correction_T_min  0.4295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         8205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0669P)^2^+0.9327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                6529
_reflns_number_total             8205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00139f.txt
_cod_data_source_block           tjm43
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

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_sg_symbol_H-M      P-1
_cod_database_code               1515496