Reactions of a tungsten trisulfido complex of hydridotris(3,5-dimethylpyrazol-1-yl)borate (Tp*) [Et(4)N][Tp*WS(3)] with CuX (X = Cl, NCS, or CN): isolation, structures, and third-order NLO properties.
Wang, Jing; Sun, Zhen-Rong; Deng, Li; Wei, Zheng-Hong; Zhang, Wen-Hua; Zhang, Yong; Lang, Jian-Ping; Inorganic chemistry 46 (2007) 11381–11389; doi:10.1021/ic701641h

data_4339196
_publ_section_title
;
 Reactions of a tungsten trisulfido complex of
 hydridotris(3,5-dimethylpyrazol-1-yl)borate (Tp*) [Et(4)N][Tp*WS(3)] with
 CuX (X = Cl, NCS, or CN): isolation, structures, and third-order NLO
 properties.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11381
_journal_page_last               11389
_journal_paper_doi               10.1021/ic701641h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C40 H50 B2 Cu8 N20 S12 W2, 2(C2 H3 N)'
_chemical_formula_sum            'C44 H56 B2 Cu8 N22 S12 W2'
_chemical_formula_weight         2175.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.876(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4069(16)
_cell_length_b                   18.823(3)
_cell_length_c                   17.893(3)
_cell_measurement_reflns_used    12354
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      3.08
_cell_volume                     3497.0(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32768
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.063
_exptl_absorpt_correction_T_max  0.5423
_exptl_absorpt_correction_T_min  0.2435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.163
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+56.9131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                5409
_reflns_number_total             6162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701641h-file003.cif
_cod_data_source_block           t
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4339196