Monomeric, Dimeric and Polymeric W/Cu/S Clusters Based on [Et4N][Tp*W(μ3-S)3(CuBr)3] and Various Nitrogen Donor Ligands
Zhen-Hong Wei; Hong-Xi Li; Mei-Ling Cheng; Xiao-Yan Tang; Yang Chen; Yong Zhang; Jian-Ping Lang; Inorganic Chemistry 48 (2009) 2808–2817; doi:10.1021/ic8019342

data_4301783
_publ_contact_author_address
;         
College of Chemistry, Chemical Engineering and Materials Science 
Suzhou University, Suzhou 215123, Jiangsu, 
P. R. China
;
_publ_contact_author_email       jplang@suda.edu.cn
_publ_contact_author_fax         86-512-65880089
_publ_contact_author_name        'Jian-Ping Lang'
_publ_contact_author_phone       86-512-65882865
_publ_section_title
;
Monomeric, Dimeric and Polymeric W/Cu/S Clusters Based on
[Et4N][Tp*W(\m3-S)3(CuBr)3] and Various Nitrogen Donor Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2808
_journal_page_last               2817
_journal_paper_doi               10.1021/ic8019342
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '2(C30 H34 B Br Cu3 N9 S3 W), F12 P2, 2(O)'
_chemical_formula_sum            'C60 H68 B2 Br2 Cu6 F12 N18 O2 P2 S6 W2'
_chemical_formula_weight         2488.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 100.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   28.987(6)
_cell_length_b                   16.351(3)
_cell_length_c                   11.547(2)
_cell_measurement_reflns_used    8666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.0677
_cell_volume                     5384.9(18)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku MercuryCCD area detector'
_diffrn_measurement_method       \w
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26599
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.237
_exptl_absorpt_correction_T_max  0.4845
_exptl_absorpt_correction_T_min  0.3630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5103
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1098P)^2^+123.8976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2261
_reflns_number_gt                4257
_reflns_number_total             5103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8019342_si_002_5.cif
_cod_data_source_block           '[Tp*W(m3-S)3Cu3(4,4'-bipy)3(m3-Br)](PF6).H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5384.9(19)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        ' C60 H68 B2 Br2 Cu6 F12 N18 O2 P2 S6 W2'
_cod_database_code               4301783