Fischer-type tungsten acyl (carbeniate), carbene and carbyne complexes bearing C5-attached thiazolyl substituents: interaction with gold(i) fragments
Strasser, Christoph E.; Cronje, Stephanie; Raubenheimer, Helgard G.; New Journal of Chemistry 34 (2010) 458–; doi:10.1039/b9nj00413k

data_7053304
_publ_section_title
;
 Fischer-type tungsten acyl (carbeniate), carbene and carbyne complexes
 bearing C5-attached thiazolyl substituents: interaction with gold(i)
 fragments
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              458
_journal_paper_doi               10.1039/b9nj00413k
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety
'C14 H12 N2 O6 S W, C14 H11 N2 O6 S W, C4 H12 N, 2(C H Cl3)'
_chemical_formula_sum            'C34 H37 Cl6 N5 O12 S2 W2'
_chemical_formula_weight         1352.2
_chemical_name_common
;
cocrystallisate of pentacarbonyl(hydroxy(2-(1- piperidyl)thiazol-5-
yl)methylidene)tungsten and tetramethylammonium pentacarbonyl((2-(1-
piperidyl)thiazol-5-yl)carbonyl)tungstate(1-) bis- trichloromethane solvate
;
_chemical_name_systematic
;cocrystallisate of pentacarbonyl{hydroxy[2-(1-piperidyl)thiazol-
5-yl]methylidene}tungsten and tetramethylammonium
pentacarbonyl{[2-(1-piperidyl)thiazol-5-yl]carbonyl}tungstate(1-)
bis-trichloromethane solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 111.940(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.273(7)
_cell_length_b                   11.491(3)
_cell_length_c                   16.925(5)
_cell_measurement_reflns_used    2833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.157
_cell_measurement_theta_min      2.507
_cell_volume                     4740(2)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'X-Seed (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  X-Seed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       \w-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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13592
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.336
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.446
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5220
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                4051
_reflns_number_total             5220
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b9nj00413k.txt
_cod_data_source_block           Compound-4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7053304