#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317698.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_4317698
loop_
_publ_author_name
'Pierre Braunstein'
'Claudia Graiff'
'Chiara Massera'
'Giovanni Predieri'
'Jacky Rosé'
'Antonio Tiripicchio'
_publ_contact_author
;
 Prof. Antonio Tiripicchio
 Dipartimento di Chimica Generale e Inorganica,
 Chimica Analitica, Chimica Fisica,
 Centro di studio per la Strutturistica Diffrattometrica del CNR
 Parco Area delle Scienze 43100 Parma, Italy
;
_publ_contact_author_email       TIRI@IPRUNIV.CCE.UNIPR.IT
_publ_section_title
;
 Reactivity of the Heterometallic Clusters [HMCo3(CO)12] and
 [Et4N][MCo3(CO)12] (M = Fe, Ru) toward Phosphine Selenides, Including
 Selenium Transfer. Crystal Structures of [HRuCo3(CO)7(μ-CO)3(μ-dppy)],
 [MCo2(μ3-Se)(CO)7(μ-dppy)], and [RuCo2(μ3-Se)(CO)7(μ-dppm)] [dppy =
 Ph2(2-C5H4N)P, dppm = Ph2PCH2PPh2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1372
_journal_page_last               1382
_journal_paper_doi               10.1021/ic010824x
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H22 Co2 O7 P2 Ru Se'
_chemical_formula_weight         878.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.798(4)
_cell_length_b                   27.858(5)
_cell_length_c                   11.272(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_volume                     6531(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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    0.1359
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9490
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         3.01
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.5891
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.986
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         9490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0477P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                3955
_reflns_number_total             9490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010824x_4.cif
_cod_data_source_block           ch83h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4317698
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.17371(3) 0.591247(19) 1.03120(5) 0.04154(15) Uani 1 d . . .
Ru1 Ru 0.229005(19) 0.663073(16) 0.95430(4) 0.03892(12) Uani 1 d . . .
Co1 Co 0.10927(3) 0.63718(2) 0.90891(6) 0.02885(16) Uani 1 d . . .
Co2 Co 0.13990(3) 0.66129(3) 1.12145(6) 0.04146(19) Uani 1 d . . .
P1 P 0.27254(6) 0.62655(5) 0.78869(12) 0.0350(3) Uani 1 d . . .
P2 P 0.13181(6) 0.59622(5) 0.74627(12) 0.0332(3) Uani 1 d . . .
O1 O -0.02532(19) 0.60614(16) 0.9338(4) 0.0700(13) Uani 1 d . . .
O2 O 0.09172(18) 0.73523(15) 0.8256(4) 0.0608(11) Uani 1 d . . .
O3 O 0.1878(2) 0.63862(19) 1.3587(4) 0.0855(15) Uani 1 d . . .
O4 O 0.0054(2) 0.6817(2) 1.1663(4) 0.106(2) Uani 1 d . . .
O5 O 0.1818(2) 0.76057(15) 1.1031(4) 0.0658(13) Uani 1 d . . .
O6 O 0.2529(2) 0.76102(15) 0.8453(4) 0.0684(13) Uani 1 d . . .
O7 O 0.34582(19) 0.66401(16) 1.1129(4) 0.0736(14) Uani 1 d . . .
C1 C 0.0279(3) 0.61778(19) 0.9249(5) 0.0426(13) Uani 1 d . . .
C2 C 0.1023(2) 0.6962(2) 0.8556(5) 0.0408(13) Uani 1 d . . .
C3 C 0.1698(3) 0.6478(2) 1.2675(6) 0.0551(16) Uani 1 d . . .
C4 C 0.0582(3) 0.6732(3) 1.1461(5) 0.0653(19) Uani 1 d . . .
C5 C 0.1738(3) 0.7205(2) 1.0954(5) 0.0527(15) Uani 1 d . . .
C6 C 0.2431(2) 0.7246(2) 0.8842(5) 0.0449(14) Uani 1 d . . .
C7 C 0.3031(3) 0.6629(2) 1.0492(5) 0.0456(14) Uani 1 d . . .
C8 C 0.2082(2) 0.61488(18) 0.6800(4) 0.0367(12) Uani 1 d . . .
H8A H 0.2010 0.6438 0.6339 0.031(9) Uiso 1 calc R . .
H8B H 0.2225 0.5900 0.6258 0.031(9) Uiso 1 calc R . .
C9 C 0.3172(2) 0.57056(19) 0.7982(5) 0.0365(12) Uani 1 d . . .
C10 C 0.3188(3) 0.5424(2) 0.8967(5) 0.0570(17) Uani 1 d . . .
H10 H 0.2968 0.5523 0.9643 0.062(8) Uiso 1 calc R . .
C11 C 0.3524(3) 0.4994(2) 0.8988(6) 0.0691(19) Uani 1 d . . .
H11 H 0.3531 0.4810 0.9677 0.062(8) Uiso 1 calc R . .
C12 C 0.3840(3) 0.4840(2) 0.8010(6) 0.0643(18) Uani 1 d . . .
H12 H 0.4055 0.4547 0.8019 0.062(8) Uiso 1 calc R . .
C13 C 0.3842(3) 0.5117(2) 0.7010(6) 0.0526(16) Uani 1 d . . .
H13 H 0.4070 0.5018 0.6344 0.062(8) Uiso 1 calc R . .
C14 C 0.3509(2) 0.55428(19) 0.6983(5) 0.0448(14) Uani 1 d . . .
H14 H 0.3507 0.5725 0.6293 0.062(8) Uiso 1 calc R . .
C15 C 0.3297(2) 0.66408(18) 0.7084(5) 0.0416(13) Uani 1 d . . .
C16 C 0.3235(3) 0.6770(2) 0.5913(6) 0.0586(17) Uani 1 d . . .
H16 H 0.2883 0.6666 0.5472 0.058(8) Uiso 1 calc R . .
C17 C 0.3705(3) 0.7061(3) 0.5391(7) 0.079(2) Uani 1 d . . .
H17 H 0.3669 0.7146 0.4595 0.058(8) Uiso 1 calc R . .
C18 C 0.4215(3) 0.7221(3) 0.6034(8) 0.087(3) Uani 1 d . . .
H18 H 0.4520 0.7418 0.5679 0.058(8) Uiso 1 calc R . .
C19 C 0.4281(3) 0.7094(3) 0.7194(8) 0.085(2) Uani 1 d . . .
H19 H 0.4629 0.7206 0.7633 0.058(8) Uiso 1 calc R . .
C20 C 0.3831(3) 0.6800(2) 0.7714(6) 0.0612(17) Uani 1 d . . .
H20 H 0.3884 0.6706 0.8500 0.058(8) Uiso 1 calc R . .
C21 C 0.1366(3) 0.53081(18) 0.7662(4) 0.0419(13) Uani 1 d . . .
C22 C 0.1857(3) 0.5029(2) 0.7225(5) 0.0527(16) Uani 1 d . . .
H22 H 0.2185 0.5167 0.6782 0.075(9) Uiso 1 calc R . .
C23 C 0.1860(4) 0.4540(2) 0.7449(7) 0.077(2) Uani 1 d . . .
H23 H 0.2198 0.4355 0.7166 0.075(9) Uiso 1 calc R . .
C24 C 0.1378(5) 0.4326(2) 0.8074(6) 0.091(3) Uani 1 d . . .
H24 H 0.1392 0.3998 0.8227 0.075(9) Uiso 1 calc R . .
C25 C 0.0874(5) 0.4599(3) 0.8475(6) 0.098(3) Uani 1 d . . .
H25 H 0.0534 0.4453 0.8875 0.075(9) Uiso 1 calc R . .
C26 C 0.0869(4) 0.5090(2) 0.8286(6) 0.079(2) Uani 1 d . . .
H26 H 0.0532 0.5275 0.8578 0.075(9) Uiso 1 calc R . .
C27 C 0.0752(2) 0.60410(18) 0.6231(4) 0.0350(12) Uani 1 d . . .
C28 C 0.0332(3) 0.5692(2) 0.5864(5) 0.0575(16) Uani 1 d . . .
H28 H 0.0337 0.5393 0.6234 0.083(10) Uiso 1 calc R . .
C29 C -0.0093(3) 0.5775(3) 0.4961(6) 0.080(2) Uani 1 d . . .
H29 H -0.0375 0.5532 0.4739 0.083(10) Uiso 1 calc R . .
C30 C -0.0115(3) 0.6196(3) 0.4387(6) 0.071(2) Uani 1 d . . .
H30 H -0.0400 0.6243 0.3762 0.083(10) Uiso 1 calc R . .
C31 C 0.0290(3) 0.6555(3) 0.4742(5) 0.0662(19) Uani 1 d . . .
H31 H 0.0279 0.6851 0.4362 0.083(10) Uiso 1 calc R . .
C32 C 0.0715(3) 0.6477(2) 0.5665(5) 0.0557(16) Uani 1 d . . .
H32 H 0.0982 0.6726 0.5909 0.083(10) Uiso 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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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
Co2 Se1 Co1 67.56(3) . . ?
Co2 Se1 Ru1 67.12(3) . . ?
Co1 Se1 Ru1 67.12(3) . . ?
C7 Ru1 C6 96.4(2) . . ?
C7 Ru1 P1 97.93(17) . . ?
C6 Ru1 P1 90.05(16) . . ?
C7 Ru1 Se1 100.41(17) . . ?
C6 Ru1 Se1 160.98(16) . . ?
P1 Ru1 Se1 96.28(4) . . ?
C7 Ru1 C5 90.9(2) . . ?
C6 Ru1 C5 76.3(2) . . ?
P1 Ru1 C5 164.50(14) . . ?
Se1 Ru1 C5 94.59(15) . . ?
C7 Ru1 Co1 152.10(17) . . ?
C6 Ru1 Co1 108.03(16) . . ?
P1 Ru1 Co1 95.31(4) . . ?
Se1 Ru1 Co1 53.62(2) . . ?
C5 Ru1 Co1 82.32(14) . . ?
C7 Ru1 Co2 99.74(17) . . ?
C6 Ru1 Co2 114.79(16) . . ?
P1 Ru1 Co2 147.38(4) . . ?
Se1 Ru1 Co2 53.64(2) . . ?
C5 Ru1 Co2 41.03(15) . . ?
Co1 Ru1 Co2 58.14(3) . . ?
C2 Co1 C1 103.9(2) . . ?
C2 Co1 P2 102.53(18) . . ?
C1 Co1 P2 97.40(17) . . ?
C2 Co1 Se1 140.42(17) . . ?
C1 Co1 Se1 108.79(17) . . ?
P2 Co1 Se1 94.93(5) . . ?
C2 Co1 Co2 95.44(18) . . ?
C1 Co1 Co2 102.71(17) . . ?
P2 Co1 Co2 148.91(5) . . ?
Se1 Co1 Co2 56.24(3) . . ?
C2 Co1 Ru1 83.60(17) . . ?
C1 Co1 Ru1 162.97(17) . . ?
P2 Co1 Ru1 95.84(4) . . ?
Se1 Co1 Ru1 59.26(2) . . ?
Co2 Co1 Ru1 60.94(2) . . ?
C4 Co2 C3 103.3(3) . . ?
C4 Co2 C5 103.3(3) . . ?
C3 Co2 C5 101.8(3) . . ?
C4 Co2 Se1 121.7(2) . . ?
C3 Co2 Se1 96.98(19) . . ?
C5 Co2 Se1 125.25(19) . . ?
C4 Co2 Co1 87.53(19) . . ?
C3 Co2 Co1 152.19(19) . . ?
C5 Co2 Co1 100.52(19) . . ?
Se1 Co2 Co1 56.21(3) . . ?
C4 Co2 Ru1 142.1(2) . . ?
C3 Co2 Ru1 114.47(19) . . ?
C5 Co2 Ru1 66.15(18) . . ?
Se1 Co2 Ru1 59.24(2) . . ?
Co1 Co2 Ru1 60.92(3) . . ?
C9 P1 C15 100.8(2) . . ?
C9 P1 C8 105.0(2) . . ?
C15 P1 C8 104.2(2) . . ?
C9 P1 Ru1 122.03(18) . . ?
C15 P1 Ru1 113.82(18) . . ?
C8 P1 Ru1 109.27(16) . . ?
C27 P2 C21 104.3(2) . . ?
C27 P2 C8 102.4(2) . . ?
C21 P2 C8 106.5(2) . . ?
C27 P2 Co1 115.49(16) . . ?
C21 P2 Co1 114.95(17) . . ?
C8 P2 Co1 112.08(17) . . ?
O1 C1 Co1 178.4(5) . . ?
O2 C2 Co1 173.2(5) . . ?
O3 C3 Co2 178.8(6) . . ?
O4 C4 Co2 177.4(6) . . ?
O5 C5 Co2 160.0(5) . . ?
O5 C5 Ru1 127.2(5) . . ?
Co2 C5 Ru1 72.8(2) . . ?
O6 C6 Ru1 177.9(5) . . ?
O7 C7 Ru1 175.5(5) . . ?
P2 C8 P1 114.1(3) . . ?
C10 C9 C14 117.3(5) . . ?
C10 C9 P1 123.7(4) . . ?
C14 C9 P1 119.1(4) . . ?
C9 C10 C11 121.6(6) . . ?
C12 C11 C10 120.3(6) . . ?
C11 C12 C13 119.5(6) . . ?
C12 C13 C14 120.3(6) . . ?
C13 C14 C9 121.0(5) . . ?
C20 C15 C16 118.8(5) . . ?
C20 C15 P1 116.7(5) . . ?
C16 C15 P1 124.4(4) . . ?
C15 C16 C17 119.3(6) . . ?
C18 C17 C16 120.7(7) . . ?
C19 C18 C17 120.4(7) . . ?
C18 C19 C20 119.7(7) . . ?
C15 C20 C19 121.1(6) . . ?
C22 C21 C26 119.1(5) . . ?
C22 C21 P2 123.9(4) . . ?
C26 C21 P2 117.0(5) . . ?
C21 C22 C23 119.7(6) . . ?
C24 C23 C22 121.5(7) . . ?
C23 C24 C25 119.3(7) . . ?
C26 C25 C24 120.1(7) . . ?
C25 C26 C21 120.3(7) . . ?
C28 C27 C32 116.8(5) . . ?
C28 C27 P2 123.5(4) . . ?
C32 C27 P2 119.5(4) . . ?
C27 C28 C29 121.1(6) . . ?
C30 C29 C28 122.0(6) . . ?
C29 C30 C31 118.5(6) . . ?
C32 C31 C30 120.1(7) . . ?
C27 C32 C31 121.5(6) . . ?
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
Se1 Co2 2.3102(10) . ?
Se1 Co1 2.3094(9) . ?
Se1 Ru1 2.4653(8) . ?
Ru1 C7 1.876(5) . ?
Ru1 C6 1.911(6) . ?
Ru1 P1 2.3108(14) . ?
Ru1 C5 2.530(6) . ?
Ru1 Co1 2.6427(8) . ?
Ru1 Co2 2.6433(9) . ?
Co1 C2 1.756(6) . ?
Co1 C1 1.786(6) . ?
Co1 P2 2.2097(15) . ?
Co1 Co2 2.5685(11) . ?
Co2 C4 1.753(7) . ?
Co2 C3 1.799(7) . ?
Co2 C5 1.816(7) . ?
P1 C9 1.819(5) . ?
P1 C15 1.824(5) . ?
P1 C8 1.843(5) . ?
P2 C27 1.833(5) . ?
P2 C21 1.839(5) . ?
P2 C8 1.831(5) . ?
O1 C1 1.157(6) . ?
O2 C2 1.160(6) . ?
O3 C3 1.124(7) . ?
O4 C4 1.146(7) . ?
O5 C5 1.133(7) . ?
O6 C6 1.123(6) . ?
O7 C7 1.143(6) . ?
C9 C10 1.360(7) . ?
C9 C14 1.401(7) . ?
C10 C11 1.388(8) . ?
C11 C12 1.354(8) . ?
C12 C13 1.367(8) . ?
C13 C14 1.373(7) . ?
C15 C20 1.390(7) . ?
C15 C16 1.375(8) . ?
C16 C17 1.401(8) . ?
C17 C18 1.359(9) . ?
C18 C19 1.362(10) . ?
C19 C20 1.376(8) . ?
C21 C22 1.374(7) . ?
C21 C26 1.390(8) . ?
C22 C23 1.383(8) . ?
C23 C24 1.363(10) . ?
C24 C25 1.373(10) . ?
C25 C26 1.386(8) . ?
C27 C28 1.372(7) . ?
C27 C32 1.375(7) . ?
C28 C29 1.368(8) . ?
C29 C30 1.341(9) . ?
C30 C31 1.367(9) . ?
C31 C32 1.383(7) . ?
