Molybdenum and Tungsten η2-Alkyne-1-thio Complexes Acting as Sulfur Donors in Homoleptic Werner Type Complexes with Nickel(II) and Palladium(II)
Seidel, Wolfram W.; Ibarra Arias, Maria D.; Schaffrath, Markus; Jahnke, Mareike C.; Hepp, Alexander; Pape, Tania; Inorganic Chemistry 45 (2006) 4791–4800; doi:10.1021/ic052178y

data_4332107
_publ_section_title
;
 Molybdenum and Tungsten \h2-Alkyne-1-thio Complexes Acting as Sulfur
 Donors in Homoleptic Werner Type Complexes with Nickel(II) and
 Palladium(II)
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4791
_journal_page_last               4800
_journal_paper_doi               10.1021/ic052178y
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C47 H50 B N6 O2 S2 W'
_chemical_formula_weight         989.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 108.4900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0754(5)
_cell_length_b                   17.8315(8)
_cell_length_c                   11.7455(6)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(1)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     2199.89(18)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
  ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(1)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25485
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    2.766
_exptl_absorpt_correction_T_max  0.8299
_exptl_absorpt_correction_T_min  0.6077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =   0.720602

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         12324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                11744
_reflns_number_total             12324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052178ysup3.cif
_cod_data_source_block           tom
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4332107