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_4339197
_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
'C8 H20 N, C15 H22 B Cl3 Cu3 N6 S3 W, 2(C H Cl3)'
_chemical_formula_sum            'C25 H44 B Cl9 Cu3 N7 S3 W'
_chemical_formula_weight         1243.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.93(3)
_cell_angle_beta                 85.13(3)
_cell_angle_gamma                75.46(3)
_cell_formula_units_Z            2
_cell_length_a                   10.355(2)
_cell_length_b                   10.390(2)
_cell_length_c                   21.624(4)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.2080
_cell_volume                     2235.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15451
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.679
_exptl_absorpt_correction_T_max  0.5011
_exptl_absorpt_correction_T_min  0.1321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.216
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8090
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1118P)^2^+32.8678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2128
_reflns_number_gt                6354
_reflns_number_total             8090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701641h-file002.cif
_cod_data_source_block           t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339197