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_4315828
_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            'C88 H170 Er2 N12 S2 Si8'
_chemical_formula_weight         2019.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A e a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.329(5)
_cell_length_b                   21.163(5)
_cell_length_c                   29.585(7)
_cell_measurement_reflns_used    1004
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.901
_cell_measurement_theta_min      2.417
_cell_volume                     12102(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1268
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10644
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.083(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10644
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                5340
_reflns_number_total             10644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100617n_si_001_12.cif
_cod_data_source_block           f80430c-Complex6-Er
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

2021-04-13
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_sg_symbol_H-M   'A b a 2'
_cod_database_code               4315828