Fast Synthesis of Hydrazine and Azo Derivatives by Oxidation of Rare-Earth-Metal−Nitrogen Bonds
Zhang, Lijun; Xia, Jing; Li, Qinghai; Li, Xihong; Wang, Shaowu; Organometallics 30 (2011) 375–; doi:10.1021/om1009928

data_4063857
_publ_section_title
;
 Fast Synthesis of Hydrazine and Azo Derivatives by Oxidation of
 Rare-Earth-Metal&#x2212;Nitrogen Bonds
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              375
_journal_paper_doi               10.1021/om1009928
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C28 H54 N3 O Si4 Yb'
_chemical_formula_weight         734.14
_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                100.6560(10)
_cell_angle_beta                 100.7260(10)
_cell_angle_gamma                102.2650(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3442(11)
_cell_length_b                   10.8748(13)
_cell_length_c                   19.243(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1825.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16025
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.713140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2004/1 - Bruker Nonius area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         8280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                7377
_reflns_number_total             8280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1009928_si_003.cif
_cod_data_source_block           COMPLEX_4
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063857