Activation of Bis(guanidinate)lanthanide Alkyl and Aryl Complexes on Elemental Sulfur: Synthesis and Characterization of Bis(guanidinate)lanthanide Thiolates and Disulfides
Zhengxing Zhang; Lixin Zhang; Yanrong Li; Longcheng Hong; Zhenxia Chen; Xigeng Zhou; Inorganic Chemistry 49 (2010) 5715–5722; doi:10.1021/ic100617n

data_4315822
_publ_contact_author_address
;Department of Chemistry
Molecular Catalysis and Innovative Material Laboratory 
Fudan University
Shanghai 200433
State Key Laboratory of Organometallic Chemistry
Shanghai 200032
People's Republic of China
;
_publ_contact_author_email       xgzhou@fudan.edu.cn
_publ_contact_author_name        'Zhou, Xigeng'
_publ_section_title
;
 Activation of Bis(guanidinate)lanthanide Alkyl and Aryl Complexes on
 Elemental Sulfur: Synthesis and Characterization of
 Bis(guanidinate)lanthanide Thiolates and Disulfides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5715
_journal_page_last               5722
_journal_paper_doi               10.1021/ic100617n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C84 H176 Er2 N12 O2 S2 Si8'
_chemical_formula_weight         2009.73
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.368(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.958(7)
_cell_length_b                   28.393(15)
_cell_length_c                   14.333(8)
_cell_measurement_reflns_used    11836
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.631
_cell_measurement_theta_min      2.473
_cell_volume                     5679(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23547
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.8806
_exptl_absorpt_correction_T_min  0.7578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.459
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         19520
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                16304
_reflns_number_total             19520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100617n_si_001_06.cif
_cod_data_source_block           f80304c-Complex4-Er
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315822