#------------------------------------------------------------------------------
#$Date: 2016-09-06 13:38:26 +0300 (Tue, 06 Sep 2016) $
#$Revision: 186170 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/18/2241830.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241830
loop_
_publ_author_name
'Drake, Hannah F.'
'Wheeler, Kraig A.'
'Bellott, Brian J.'
_publ_section_title
;
 Crystal structure of (OC)₅W(μ-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
'[μ-Ethane-1,2-diylbis(diphenylphosphane)-κ²P:P']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/[σ²(Fo²)+(0.0218P)²+0.5664P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            vn2114sup1.cif
_cod_data_source_block           I
_cod_database_code               2241830
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.871
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
W W1 0.17092(2) 0.47944(2) 0.81902(2) 0.01462(6) Uani d 1
P P1 0.15114(8) 0.56563(5) 0.63197(7) 0.01359(16) Uani d 1
O O1 0.1345(2) 0.64362(16) 0.9701(2) 0.0277(6) Uani d 1
O O2 -0.1519(2) 0.44991(18) 0.7958(2) 0.0324(6) Uani d 1
O O3 0.2025(2) 0.36975(16) 1.0520(2) 0.0286(6) Uani d 1
O O4 0.2103(3) 0.31759(16) 0.6641(2) 0.0317(6) Uani d 1
O O5 0.4947(2) 0.50864(15) 0.8560(2) 0.0274(6) Uani d 1
C C1 0.0518(3) 0.66234(19) 0.6298(3) 0.0162(6) Uani d 1
C C2 0.0733(3) 0.7262(2) 0.5503(3) 0.0206(7) Uani d 1
H H2 0.1383 0.7188 0.4950 0.025 Uiso calc 1
C C3 0.0010(3) 0.8002(2) 0.5510(3) 0.0251(8) Uani d 1
H H3 0.0155 0.8429 0.4958 0.030 Uiso calc 1
C C4 -0.0924(3) 0.8119(2) 0.6323(3) 0.0253(8) Uani d 1
H H4 -0.1402 0.8633 0.6342 0.030 Uiso calc 1
C C5 -0.1164(3) 0.7490(2) 0.7106(3) 0.0238(7) Uani d 1
H H5 -0.1813 0.7571 0.7657 0.029 Uiso calc 1
C C6 -0.0453(3) 0.6737(2) 0.7089(3) 0.0196(7) Uani d 1
H H6 -0.0633 0.6301 0.7618 0.023 Uiso calc 1
C C7 0.3146(3) 0.60406(19) 0.5907(3) 0.0149(6) Uani d 1
C C8 0.3683(3) 0.5823(2) 0.4868(3) 0.0202(7) Uani d 1
H H8 0.3191 0.5455 0.4319 0.024 Uiso calc 1
C C9 0.4940(3) 0.6143(2) 0.4630(3) 0.0264(8) Uani d 1
H H9 0.5300 0.5991 0.3917 0.032 Uiso calc 1
C C10 0.5671(3) 0.6679(2) 0.5420(3) 0.0260(8) Uani d 1
H H10 0.6532 0.6892 0.5256 0.031 Uiso calc 1
C C11 0.5130(4) 0.6903(2) 0.6460(3) 0.0269(8) Uani d 1
H H11 0.5614 0.7280 0.7001 0.032 Uiso calc 1
C C12 0.3894(3) 0.6578(2) 0.6706(3) 0.0218(7) Uani d 1
H H12 0.3546 0.6722 0.7428 0.026 Uiso calc 1
C C13 0.0738(3) 0.51389(19) 0.4953(3) 0.0146(6) Uani d 1
H H13A 0.0747 0.5528 0.4275 0.018 Uiso calc 1
H H13B 0.1297 0.4647 0.4793 0.018 Uiso calc 1
C C14 0.1472(3) 0.5850(2) 0.9158(3) 0.0205(7) Uani d 1
C C15 -0.0363(4) 0.4607(2) 0.8030(3) 0.0213(7) Uani d 1
C C16 0.1906(3) 0.4096(2) 0.9678(3) 0.0207(7) Uani d 1
C C17 0.1959(3) 0.3754(2) 0.7191(3) 0.0202(7) Uani d 1
C C18 0.3793(4) 0.4984(2) 0.8413(3) 0.0205(7) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle
C16 W1 C15 . 89.55(13)
C16 W1 C14 . 91.03(13)
C15 W1 C14 . 89.83(13)
C16 W1 C17 . 90.16(13)
C15 W1 C17 . 90.64(13)
C14 W1 C17 . 178.72(13)
C16 W1 C18 . 88.85(13)
C15 W1 C18 . 178.03(12)
C14 W1 C18 . 89.05(13)
C17 W1 C18 . 90.52(13)
C16 W1 P1 . 178.79(9)
C15 W1 P1 . 91.45(9)
C14 W1 P1 . 89.64(9)
C17 W1 P1 . 89.16(9)
C18 W1 P1 . 90.16(9)
C7 P1 C1 . 101.08(14)
C7 P1 C13 . 103.13(14)
C1 P1 C13 . 101.69(14)
C7 P1 W1 . 114.44(10)
C1 P1 W1 . 117.80(11)
C13 P1 W1 . 116.38(10)
C6 C1 C2 . 118.9(3)
C6 C1 P1 . 120.3(2)
C2 C1 P1 . 120.7(2)
C3 C2 C1 . 120.7(3)
C3 C2 H2 . 119.6
C1 C2 H2 . 119.6
C2 C3 C4 . 120.0(3)
C2 C3 H3 . 120.0
C4 C3 H3 . 120.0
C5 C4 C3 . 120.1(3)
C5 C4 H4 . 119.9
C3 C4 H4 . 119.9
C4 C5 C6 . 120.2(3)
C4 C5 H5 . 119.9
C6 C5 H5 . 119.9
C1 C6 C5 . 120.1(3)
C1 C6 H6 . 120.0
C5 C6 H6 . 120.0
C8 C7 C12 . 118.8(3)
C8 C7 P1 . 124.1(2)
C12 C7 P1 . 117.0(2)
C7 C8 C9 . 120.2(3)
C7 C8 H8 . 119.9
C9 C8 H8 . 119.9
C10 C9 C8 . 120.7(3)
C10 C9 H9 . 119.6
C8 C9 H9 . 119.6
C9 C10 C11 . 119.2(3)
C9 C10 H10 . 120.4
C11 C10 H10 . 120.4
C12 C11 C10 . 120.2(3)
C12 C11 H11 . 119.9
C10 C11 H11 . 119.9
C11 C12 C7 . 120.8(3)
C11 C12 H12 . 119.6
C7 C12 H12 . 119.6
C13 C13 P1 3_566 112.1(3)
C13 C13 H13A 3_566 109.2
P1 C13 H13A . 109.2
C13 C13 H13B 3_566 109.2
P1 C13 H13B . 109.2
H13A C13 H13B . 107.9
O1 C14 W1 . 179.7(3)
O2 C15 W1 . 179.0(3)
O3 C16 W1 . 179.6(3)
O4 C17 W1 . 179.6(3)
O5 C18 W1 . 178.7(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
W1 C16 . 2.015(3)
W1 C15 . 2.044(4)
W1 C14 . 2.045(4)
W1 C17 . 2.048(3)
W1 C18 . 2.056(4)
W1 P1 . 2.5200(8)
P1 C7 . 1.829(3)
P1 C1 . 1.832(3)
P1 C13 . 1.843(3)
O1 C14 . 1.140(4)
O2 C15 . 1.143(4)
O3 C16 . 1.144(4)
O4 C17 . 1.135(4)
O5 C18 . 1.139(4)
C1 C6 . 1.393(4)
C1 C2 . 1.397(5)
C2 C3 . 1.384(5)
C2 H2 . 0.9500
C3 C4 . 1.385(5)
C3 H3 . 0.9500
C4 C5 . 1.381(5)
C4 H4 . 0.9500
C5 C6 . 1.398(5)
C5 H5 . 0.9500
C6 H6 . 0.9500
C7 C8 . 1.388(4)
C7 C12 . 1.397(5)
C8 C9 . 1.391(5)
C8 H8 . 0.9500
C9 C10 . 1.382(5)
C9 H9 . 0.9500
C10 C11 . 1.394(5)
C10 H10 . 0.9500
C11 C12 . 1.378(5)
C11 H11 . 0.9500
C12 H12 . 0.9500
C13 C13 3_566 1.531(6)
C13 H13A . 0.9900
C13 H13B . 0.9900
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
C7 P1 C1 C6 . -146.7(3)
C13 P1 C1 C6 . 107.2(3)
W1 P1 C1 C6 . -21.3(3)
C7 P1 C1 C2 . 32.5(3)
C13 P1 C1 C2 . -73.6(3)
W1 P1 C1 C2 . 157.9(2)
C6 C1 C2 C3 . 1.0(5)
P1 C1 C2 C3 . -178.1(3)
C1 C2 C3 C4 . 0.9(5)
C2 C3 C4 C5 . -1.7(5)
C3 C4 C5 C6 . 0.7(5)
C2 C1 C6 C5 . -2.1(5)
P1 C1 C6 C5 . 177.1(2)
C4 C5 C6 C1 . 1.2(5)
C1 P1 C7 C8 . -115.3(3)
C13 P1 C7 C8 . -10.3(3)
W1 P1 C7 C8 . 117.1(3)
C1 P1 C7 C12 . 65.5(3)
C13 P1 C7 C12 . 170.5(3)
W1 P1 C7 C12 . -62.2(3)
C12 C7 C8 C9 . -0.5(5)
P1 C7 C8 C9 . -179.7(3)
C7 C8 C9 C10 . 0.0(5)
C8 C9 C10 C11 . -0.5(5)
C9 C10 C11 C12 . 1.4(5)
C10 C11 C12 C7 . -1.8(5)
C8 C7 C12 C11 . 1.4(5)
P1 C7 C12 C11 . -179.4(3)
C7 P1 C13 C13 3_566 -172.8(3)
C1 P1 C13 C13 3_566 -68.3(3)
W1 P1 C13 C13 3_566 61.0(3)

_cod_database_fobs_code 2241830
