Investigations on Organolanthanide Derivatives with the Hydrazonido (−NHN═CPh2) Ligand: Synthesis, Crystal Structure, and Reactivity
Han, Yanan; Zhang, Jie; Han, Fuyan; Zhang, Zhengxing; Weng, Linhong; Zhou, Xigeng; Organometallics 28 (2009) 3916–; doi:10.1021/om900246b

data_4069527
_publ_section_title
;
 Investigations on Organolanthanide Derivatives with the Hydrazonido
 (&#x2212;NHN&#x2550;CPh2) Ligand: Synthesis, Crystal Structure, and
 Reactivity
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3916
_journal_paper_doi               10.1021/om900246b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C46 H42 Er2 N4'
_chemical_formula_weight         985.36
_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           SHELXL-97
_cell_angle_alpha                99.501(8)
_cell_angle_beta                 100.715(8)
_cell_angle_gamma                98.183(8)
_cell_formula_units_Z            2
_cell_length_a                   8.243(6)
_cell_length_b                   11.398(8)
_cell_length_c                   21.169(15)
_cell_measurement_reflns_used    1231
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.435
_cell_measurement_theta_min      2.436
_cell_volume                     1896(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0803
_diffrn_reflns_av_sigmaI/netI    0.2194
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7592
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    4.433
_exptl_absorpt_correction_T_max  0.7181
_exptl_absorpt_correction_T_min  0.4709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.729
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.458
_refine_ls_extinction_coef       0.080(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         6458
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1981
_refine_ls_R_factor_gt           0.1148
_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^)+(0.1571P)^2^+2.8169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2829
_refine_ls_wR_factor_ref         0.3270
_reflns_number_gt                3317
_reflns_number_total             6458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900246b_si_001.cif
_cod_data_source_block           2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1897(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069527