#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/27/4312709.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312709
loop_
_publ_author_name
'Daniele Belletti'
'Claudia Graiff'
'Chiara Massera'
'Alex Minarelli'
'Giovanni Predieri'
'Antonio Tiripicchio'
'Domenico Acquotti'
_publ_contact_author
;
  Dr. Claudia Graiff
  Dipartimento di Chimica GIAF, Universita' di Parma
  Parco Area delle Scienze 17/A, I-43100 Parma, Italy
;
_publ_contact_author_email       claudia.graiff@unipr.it
_publ_section_title
;
 Reactivity of Ph2P(Se)CH2C6H4CH2P(Se)Ph2 with [M3(CO)12] (M = Ru or Fe).
 Synthesis and Characterization of the New Carbene Cluster
 [Ru3(μ3-Se)(μ3-H)(μ2-PPh2)(CO)6(μ2-CHC6H4CH2PPh2)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8509
_journal_page_last               8518
_journal_paper_doi               10.1021/ic034887m
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C32 H28 P2 Se2'
_chemical_formula_weight         632.40
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                90.000(5)
_cell_angle_beta                 98.120(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   23.451(5)
_cell_length_b                   9.226(5)
_cell_length_c                   26.289(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.96
_cell_measurement_theta_min      13.51
_cell_volume                     5631(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       'θ/2θ 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8191
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.13
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.1243
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.743
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00029(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         8191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0458
_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/[σ²(Fo²)+(0.0569P)²+1.0764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                4863
_reflns_number_total             8191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034887msi20030730_124443_2.cif
_cod_data_source_block           xy
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4312709
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.62715(3) -0.17417(9) 0.11630(3) 0.03006(18) Uani 1 1 d . . .
P2 P 0.41564(3) 0.11316(9) 0.11709(3) 0.02868(17) Uani 1 1 d . . .
Se1 Se 0.665439(16) -0.24796(5) 0.052843(13) 0.04856(12) Uani 1 1 d . . .
Se2 Se 0.469343(16) 0.08011(5) 0.187857(12) 0.05282(14) Uani 1 1 d . . .
C1 C 0.55903(12) -0.0793(3) 0.09858(11) 0.0305(6) Uani 1 1 d . . .
H1A H 0.5332 -0.1457 0.0781 0.037(4) Uiso 1 1 calc R . .
H1B H 0.5429 -0.0619 0.1300 0.037(4) Uiso 1 1 calc R . .
C2 C 0.55683(12) 0.0632(3) 0.06963(10) 0.0249(6) Uani 1 1 d . . .
C3 C 0.60632(13) 0.1326(4) 0.05853(11) 0.0340(7) Uani 1 1 d . . .
H3 H 0.6421 0.0912 0.0695 0.071(4) Uiso 1 1 calc R . .
C4 C 0.60338(15) 0.2623(4) 0.03140(12) 0.0405(8) Uani 1 1 d . . .
H4 H 0.6370 0.3071 0.0244 0.071(4) Uiso 1 1 calc R . .
C5 C 0.55030(15) 0.3249(4) 0.01478(12) 0.0411(8) Uani 1 1 d . . .
H5 H 0.5480 0.4115 -0.0035 0.071(4) Uiso 1 1 calc R . .
C6 C 0.50085(14) 0.2576(3) 0.02556(11) 0.0345(7) Uani 1 1 d . . .
H6 H 0.4653 0.3002 0.0146 0.071(4) Uiso 1 1 calc R . .
C7 C 0.50308(12) 0.1269(3) 0.05265(10) 0.0265(6) Uani 1 1 d . . .
C8 C 0.44630(11) 0.0564(3) 0.05999(10) 0.0278(6) Uani 1 1 d . . .
H8A H 0.4519 -0.0478 0.0616 0.037(4) Uiso 1 1 calc R . .
H8B H 0.4184 0.0769 0.0299 0.037(4) Uiso 1 1 calc R . .
C9 C 0.67425(13) -0.0619(4) 0.16102(11) 0.0355(7) Uani 1 1 d . . .
C10 C 0.65283(17) 0.0463(4) 0.19009(13) 0.0454(8) Uani 1 1 d . . .
H10 H 0.6137 0.0673 0.1856 0.071(4) Uiso 1 1 calc R . .
C12 C 0.7483(2) 0.0933(6) 0.23294(17) 0.0737(14) Uani 1 1 d . . .
H12 H 0.7730 0.1447 0.2573 0.071(4) Uiso 1 1 calc R . .
C13 C 0.76968(18) -0.0127(6) 0.20381(17) 0.0700(14) Uani 1 1 d . . .
H13 H 0.8090 -0.0325 0.2085 0.071(4) Uiso 1 1 calc R . .
C11 C 0.6905(2) 0.1222(5) 0.22575(15) 0.0646(12) Uani 1 1 d . . .
H11 H 0.6763 0.1943 0.2452 0.071(4) Uiso 1 1 calc R . .
C14 C 0.73306(15) -0.0904(4) 0.16744(14) 0.0501(9) Uani 1 1 d . . .
H14 H 0.7478 -0.1608 0.1476 0.071(4) Uiso 1 1 calc R . .
C15 C 0.60661(13) -0.3213(4) 0.15652(12) 0.0344(7) Uani 1 1 d . . .
C16 C 0.58954(16) -0.2916(4) 0.20399(14) 0.0505(9) Uani 1 1 d . . .
H16 H 0.5885 -0.1964 0.2154 0.071(4) Uiso 1 1 calc R . .
C17 C 0.57394(19) -0.4047(5) 0.23439(16) 0.0647(12) Uani 1 1 d . . .
H17 H 0.5625 -0.3854 0.2662 0.071(4) Uiso 1 1 calc R . .
C18 C 0.57557(18) -0.5454(5) 0.2169(2) 0.0707(14) Uani 1 1 d . . .
H18 H 0.5655 -0.6212 0.2372 0.071(4) Uiso 1 1 calc R . .
C19 C 0.5918(2) -0.5741(5) 0.1702(2) 0.0749(14) Uani 1 1 d . . .
H19 H 0.5922 -0.6692 0.1585 0.071(4) Uiso 1 1 calc R . .
C20 C 0.60771(17) -0.4634(4) 0.14030(16) 0.0533(10) Uani 1 1 d . . .
H20 H 0.6193 -0.4844 0.1087 0.071(4) Uiso 1 1 calc R . .
C21 C 0.39645(14) 0.3035(4) 0.10753(11) 0.0337(7) Uani 1 1 d . . .
C22 C 0.43752(18) 0.4075(4) 0.12529(15) 0.0550(10) Uani 1 1 d . . .
H22 H 0.4736 0.3788 0.1415 0.071(4) Uiso 1 1 calc R . .
C23 C 0.4248(2) 0.5541(5) 0.11893(18) 0.0689(13) Uani 1 1 d . . .
H23 H 0.4525 0.6231 0.1305 0.071(4) Uiso 1 1 calc R . .
C24 C 0.3719(2) 0.5967(5) 0.09592(17) 0.0681(13) Uani 1 1 d . . .
H24 H 0.3635 0.6949 0.0921 0.071(4) Uiso 1 1 calc R . .
C25 C 0.3310(2) 0.4953(5) 0.07828(16) 0.0639(12) Uani 1 1 d . . .
H25 H 0.2949 0.5250 0.0625 0.071(4) Uiso 1 1 calc R . .
C26 C 0.34336(16) 0.3481(4) 0.08395(13) 0.0457(9) Uani 1 1 d . . .
H26 H 0.3156 0.2798 0.0717 0.071(4) Uiso 1 1 calc R . .
C27 C 0.34813(13) 0.0121(3) 0.11179(11) 0.0319(7) Uani 1 1 d . . .
C28 C 0.31525(14) -0.0187(4) 0.06484(13) 0.0417(8) Uani 1 1 d . . .
H28 H 0.3274 0.0130 0.0346 0.071(4) Uiso 1 1 calc R . .
C29 C 0.26464(16) -0.0959(5) 0.06289(16) 0.0572(10) Uani 1 1 d . . .
H29 H 0.2432 -0.1174 0.0313 0.071(4) Uiso 1 1 calc R . .
C30 C 0.24571(18) -0.1415(5) 0.10779(18) 0.0637(12) Uani 1 1 d . . .
H30 H 0.2114 -0.1929 0.1066 0.071(4) Uiso 1 1 calc R . .
C31 C 0.2779(2) -0.1101(5) 0.15380(18) 0.0731(14) Uani 1 1 d . . .
H31 H 0.2651 -0.1403 0.1840 0.071(4) Uiso 1 1 calc R . .
C32 C 0.32916(18) -0.0347(4) 0.15673(15) 0.0555(10) Uani 1 1 d . . .
H32 H 0.3507 -0.0154 0.1885 0.071(4) Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 P1 C1 108.79(15) . . ?
C9 P1 C15 103.57(14) . . ?
C1 P1 C15 102.21(14) . . ?
C9 P1 Se1 113.98(11) . . ?
C1 P1 Se1 114.01(10) . . ?
C15 P1 Se1 113.16(12) . . ?
C21 P2 C27 106.69(15) . . ?
C21 P2 C8 106.32(14) . . ?
C27 P2 C8 103.18(13) . . ?
C21 P2 Se2 111.41(10) . . ?
C27 P2 Se2 113.28(10) . . ?
C8 P2 Se2 115.21(9) . . ?
C2 C1 P1 120.7(2) . . ?
C3 C2 C7 118.6(3) . . ?
C3 C2 C1 122.3(3) . . ?
C7 C2 C1 119.2(2) . . ?
C4 C3 C2 121.4(3) . . ?
C5 C4 C3 119.8(3) . . ?
C6 C5 C4 119.5(3) . . ?
C5 C6 C7 121.4(3) . . ?
C6 C7 C2 119.3(3) . . ?
C6 C7 C8 117.7(3) . . ?
C2 C7 C8 122.9(3) . . ?
C7 C8 P2 115.75(19) . . ?
C14 C9 C10 119.8(3) . . ?
C14 C9 P1 118.2(3) . . ?
C10 C9 P1 122.0(3) . . ?
C11 C10 C9 119.2(4) . . ?
C11 C12 C13 119.4(4) . . ?
C12 C13 C14 120.7(4) . . ?
C12 C11 C10 121.4(4) . . ?
C9 C14 C13 119.5(4) . . ?
C20 C15 C16 119.0(3) . . ?
C20 C15 P1 120.6(3) . . ?
C16 C15 P1 120.4(3) . . ?
C15 C16 C17 119.9(4) . . ?
C18 C17 C16 119.4(4) . . ?
C19 C18 C17 120.5(4) . . ?
C18 C19 C20 120.3(4) . . ?
C19 C20 C15 120.8(4) . . ?
C26 C21 C22 119.0(3) . . ?
C26 C21 P2 122.8(3) . . ?
C22 C21 P2 118.2(3) . . ?
C23 C22 C21 120.2(4) . . ?
C24 C23 C22 120.2(4) . . ?
C23 C24 C25 120.2(4) . . ?
C24 C25 C26 120.2(4) . . ?
C21 C26 C25 120.2(4) . . ?
C28 C27 C32 119.2(3) . . ?
C28 C27 P2 122.6(2) . . ?
C32 C27 P2 118.2(3) . . ?
C29 C28 C27 120.4(3) . . ?
C28 C29 C30 120.2(4) . . ?
C31 C30 C29 119.2(4) . . ?
C30 C31 C32 121.7(4) . . ?
C31 C32 C27 119.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C9 1.819(3) . ?
P1 C1 1.823(3) . ?
P1 C15 1.826(3) . ?
P1 Se1 2.1157(9) . ?
P2 C21 1.822(4) . ?
P2 C27 1.826(3) . ?
P2 C8 1.830(3) . ?
P2 Se2 2.1162(8) . ?
C1 C2 1.516(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.405(4) . ?
C3 C4 1.390(4) . ?
C4 C5 1.385(5) . ?
C5 C6 1.379(4) . ?
C6 C7 1.398(4) . ?
C7 C8 1.519(4) . ?
C9 C14 1.391(5) . ?
C9 C10 1.393(5) . ?
C10 C11 1.384(5) . ?
C12 C11 1.368(7) . ?
C12 C13 1.379(7) . ?
C13 C14 1.390(5) . ?
C15 C20 1.380(5) . ?
C15 C16 1.391(4) . ?
C16 C17 1.394(5) . ?
C17 C18 1.379(6) . ?
C18 C19 1.363(7) . ?
C19 C20 1.371(6) . ?
C21 C26 1.373(5) . ?
C21 C22 1.392(5) . ?
C22 C23 1.390(6) . ?
C23 C24 1.357(7) . ?
C24 C25 1.374(6) . ?
C25 C26 1.392(6) . ?
C27 C28 1.389(4) . ?
C27 C32 1.388(4) . ?
C28 C29 1.379(5) . ?
C29 C30 1.384(6) . ?
C30 C31 1.363(6) . ?
C31 C32 1.382(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660913
