Bis{decacarbonylbis[μ-2,2'-(phenylimino)diethanolato]ditin(II)ditungsten(0)(2 <i>Sn{—</i>W})} hexacarbonyltungsten(0)
Berends, Thorsten; Iovkova, Ljuba; Tiekink, Edward R. T.; Jurkschat, Klaus; Acta Crystallographica Section E 66 (2010) m715–m716; doi:10.1107/S1600536810019343

data_2226153
_publ_section_title
;
 Bis{decacarbonylbis[\m-2,2'-(phenylimino)diethanolato]ditin(II)ditungsten(0)(2
 <i>Sn{---</i>W})} hexacarbonyltungsten(0)
;
_journal_coeditor_code           HB5458
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m715
_journal_page_last               m716
_journal_paper_doi               10.1107/S1600536810019343
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Sn2 W2 (C10 H13 N O2)2 (C O)10]2 [W (C O)6]'
_chemical_formula_moiety         '2(C30 H26 N2 O14 Sn2 W2), C6 O6 W'
_chemical_formula_sum            'C66 H52 N4 O34 Sn4 W5'
_chemical_formula_weight         2839.15
_chemical_melting_point          460
_chemical_name_common
;
Bis{decacarbonylbis[\m-2,2'-(phenylimino)diethanolato]ditin(II)ditungsten(0)(2
<i>Sn---W</i>)} hexacarbonyltungsten(0)
;
_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                108.715(4)
_cell_angle_beta                 92.758(4)
_cell_angle_gamma                115.350(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3547(5)
_cell_length_b                   12.5454(5)
_cell_length_c                   16.8187(7)
_cell_measurement_reflns_used    35730
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.0
_cell_volume                     2001.90(18)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2 CCD'
_diffrn_measurement_method
;
973 frames via \w-rotation (\D\w = 1\%) and two times 30 s
per frame (16 sets at different \k-angles)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39646
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.95
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9035
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.95
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.020
_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^)+(0.018P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.038
_refine_ls_wR_factor_ref         0.039
_reflns_number_gt                7218
_reflns_number_total             9035
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5458.cif
_cod_data_source_block           I
_cod_original_cell_volume        2001.90(19)
_cod_database_code               2226153
_cod_database_fobs_code          2226153