Crystal structure of (OC)~5~W(μ-dppe)W(CO)~5~
Drake, Hannah F.; Wheeler, Kraig A.; Bellott, Brian J.; Acta Crystallographica Section E 72 (2016) 1383–1385; doi:10.1107/S2056989016013670

data_2241830
_publ_section_title
;
 Crystal structure of (OC)~5~W(\m-dppe)W(CO)~5~
;
_journal_coeditor_code           VN2114
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1383
_journal_page_last               1385
_journal_paper_doi               10.1107/S2056989016013670
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[W2 (C26 H24 P2) (C O)10]'
_chemical_formula_moiety         'C36 H24 O10 P2 W2'
_chemical_formula_sum            'C36 H24 O10 P2 W2'
_chemical_formula_weight         1046.17
_chemical_name_systematic
'[\m-Ethane-1,2-diylbis(diphenylphosphane)-\k^2^<i>P</i>:<i>P</i>']bis[pentacarbonyltungsten(0)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.511(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8193(4)
_cell_length_b                   16.0492(7)
_cell_length_c                   11.3312(5)
_cell_measurement_reflns_used    8094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.604
_cell_measurement_theta_min      4.591
_cell_volume                     1774.19(13)
_computing_cell_refinement
;
SAINT (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_molecular_graphics
;
XSEED (Barbour, 2001)
;
_computing_publication_material
;
XSEED (Barbour, 2001)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26419
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.237
_diffrn_reflns_theta_min         4.798
_exptl_absorpt_coefficient_mu    13.150
_exptl_absorpt_correction_T_max  .756
_exptl_absorpt_correction_T_min  .254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2011)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       'transparent rhomboid'
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.579
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.5664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0478
_reflns_number_gt                2954
_reflns_number_total             3256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vn2114sup1.cif
_cod_data_source_block           I
_cod_database_code               2241830
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.871
_shelx_hkl_checksum              21222
_shelx_res_checksum              8295
_cod_database_fobs_code 2241830