Double-Stranded W/Ag/S Chain Structure Generated from [syn-{WO(NCS)2}2(μ-S)2] Building Blocks
Wenjian Zhang; Xintao Wu; Biao Wu; Shuyan Yu; Gabriella Santoni; Dieter Rehder; Inorganic Chemistry 42 (2003) 1130–1134; doi:10.1021/ic020510p

data_4313094
_publ_contact_author_address
; 
Institute of Inorganic and Applied Chemistry 
Martin-Luther-King-Platz 6 
20146 Hamburg 
Germany 
;
_publ_contact_author_email       rehder@xray.chemie.uni-hamburg.de
_publ_contact_author_fax         +49-40-42838-2893
_publ_contact_author_name        'Professor Dieter Rehder'
_publ_contact_author_phone       +49-40-42838-6087
_publ_section_title
;
 Double-Stranded W/Ag/S Chain Structure Generated from
 [syn-{WO(NCS)2}2(\m-S)2] Building Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1130
_journal_page_last               1134
_journal_paper_doi               10.1021/ic020510p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C38 H80 N10 O2 S8 W2'
_chemical_formula_weight         1333.30
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   15.2671(11)
_cell_length_b                   18.9237(14)
_cell_length_c                   19.2443(14)
_cell_measurement_reflns_used    5140
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.753
_cell_measurement_theta_min      2.669
_cell_volume                     5559.9(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics
; 
ASp 
Copyright, 
Chen, Jiutong, 
Fujian Institute 
;
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26995
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    4.475
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker sadabs'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9232
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0584P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                8395
_reflns_number_total             9232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020510p_1.cif
_cod_data_source_block           1
_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 
;
_cod_database_code               4313094