#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317695.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_4317695
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            'C24 H14 Co2 Fe N O7 P Se'
_chemical_formula_weight         712.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 115.96(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.206(4)
_cell_length_b                   21.226(5)
_cell_length_c                   11.276(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_volume                     2626.7(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7981
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.42
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.284
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7515
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.21
_exptl_crystal_density_meas      0.27
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0393P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                4500
_reflns_number_total             7668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010824x_1.cif
_cod_data_source_block           cm15h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0393P)^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^)+(0.0393P)^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_original_cell_volume        2626.7(14)
_cod_database_code               4317695
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54119(4) 0.66545(2) 0.34834(4) 0.04043(12) Uani 1 d . . .
Co1 Co 0.60710(3) 0.637483(18) 0.59061(4) 0.03187(10) Uani 1 d . . .
Co2 Co 0.71904(4) 0.58967(2) 0.47103(4) 0.03690(10) Uani 1 d . . .
Se1 Se 0.51983(3) 0.566955(15) 0.41983(3) 0.03865(8) Uani 1 d . . .
P1 P 0.83159(7) 0.54556(4) 0.66338(8) 0.03491(17) Uani 1 d . . .
O1 O 0.3959(2) 0.70044(15) 0.5920(3) 0.0789(9) Uani 1 d . . .
O2 O 0.7777(2) 0.74196(12) 0.7022(2) 0.0619(7) Uani 1 d . . .
O3 O 0.8781(2) 0.69537(13) 0.4860(3) 0.0676(7) Uani 1 d . . .
O4 O 0.7339(3) 0.50659(16) 0.2724(3) 0.0947(11) Uani 1 d . . .
O5 O 0.5256(3) 0.64171(17) 0.0861(3) 0.0991(11) Uani 1 d . . .
O6 O 0.2920(3) 0.71203(17) 0.2578(3) 0.0902(10) Uani 1 d . . .
O7 O 0.6553(3) 0.79048(12) 0.4071(3) 0.0668(8) Uani 1 d . . .
N1 N 0.6574(2) 0.57500(11) 0.7409(2) 0.0346(5) Uani 1 d . . .
C1 C 0.4782(3) 0.67470(16) 0.5926(3) 0.0446(8) Uani 1 d . . .
C2 C 0.7144(3) 0.70018(15) 0.6614(3) 0.0387(7) Uani 1 d . . .
C3 C 0.8147(3) 0.65438(18) 0.4776(3) 0.0483(8) Uani 1 d . . .
C4 C 0.7312(3) 0.53900(19) 0.3517(4) 0.0588(10) Uani 1 d . . .
C5 C 0.5330(4) 0.65167(18) 0.1893(4) 0.0588(10) Uani 1 d . . .
C6 C 0.3893(4) 0.6931(2) 0.2937(4) 0.0597(10) Uani 1 d . . .
C7 C 0.6130(3) 0.74119(17) 0.3839(3) 0.0493(8) Uani 1 d . . .
C8 C 0.7494(3) 0.53359(14) 0.7653(3) 0.0356(7) Uani 1 d . . .
C9 C 0.7790(3) 0.48726(16) 0.8606(3) 0.0486(8) Uani 1 d . . .
H9 H 0.8420 0.4592 0.8744 0.068(6) Uiso 1 calc R . .
C10 C 0.7153(3) 0.48258(18) 0.9350(3) 0.0564(10) Uani 1 d . . .
H10 H 0.7338 0.4515 0.9990 0.068(6) Uiso 1 calc R . .
C11 C 0.6245(3) 0.52482(18) 0.9124(3) 0.0552(9) Uani 1 d . . .
H11 H 0.5812 0.5234 0.9627 0.068(6) Uiso 1 calc R . .
C12 C 0.5965(3) 0.56956(16) 0.8156(3) 0.0458(8) Uani 1 d . . .
H12 H 0.5329 0.5973 0.8008 0.068(6) Uiso 1 calc R . .
C13 C 0.8989(3) 0.46760(15) 0.6727(3) 0.0404(7) Uani 1 d . . .
C14 C 1.0141(3) 0.45142(17) 0.7705(4) 0.0542(9) Uani 1 d . . .
H14 H 1.0623 0.4817 0.8300 0.069(5) Uiso 1 calc R . .
C15 C 1.0566(3) 0.39031(18) 0.7789(4) 0.0647(11) Uani 1 d . . .
H15 H 1.1331 0.3797 0.8445 0.069(5) Uiso 1 calc R . .
C16 C 0.9868(4) 0.34529(18) 0.6912(4) 0.0653(11) Uani 1 d . . .
H16 H 1.0160 0.3044 0.6973 0.069(5) Uiso 1 calc R . .
C17 C 0.8300(3) 0.42199(17) 0.5849(4) 0.0575(10) Uani 1 d . . .
H17 H 0.7536 0.4322 0.5187 0.069(5) Uiso 1 calc R . .
C18 C 0.8740(4) 0.36062(18) 0.5947(4) 0.0719(12) Uani 1 d . . .
H18 H 0.8266 0.3300 0.5354 0.069(5) Uiso 1 calc R . .
C19 C 0.9615(3) 0.59444(14) 0.7696(3) 0.0398(7) Uani 1 d . . .
C20 C 0.9703(3) 0.62297(16) 0.8850(3) 0.0505(8) Uani 1 d . . .
H20 H 0.9116 0.6151 0.9149 0.073(6) Uiso 1 calc R . .
C21 C 1.0672(4) 0.66331(19) 0.9551(4) 0.0650(11) Uani 1 d . . .
H21 H 1.0724 0.6827 1.0314 0.073(6) Uiso 1 calc R . .
C22 C 1.1542(4) 0.67474(19) 0.9136(5) 0.0717(13) Uani 1 d . . .
H22 H 1.2191 0.7013 0.9620 0.073(6) Uiso 1 calc R . .
C23 C 1.1465(3) 0.6469(2) 0.7997(4) 0.0686(12) Uani 1 d . . .
H23 H 1.2059 0.6551 0.7712 0.073(6) Uiso 1 calc R . .
C24 C 1.0515(3) 0.60706(17) 0.7279(4) 0.0517(9) Uani 1 d . . .
H24 H 1.0471 0.5885 0.6513 0.073(6) 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'
N N 0.0061 0.0033 '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'
Se Se -0.0929 2.2259 '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'
Fe Fe 0.3463 0.8444 '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
C5 Fe1 C6 96.62(19) . . ?
C5 Fe1 C7 100.35(17) . . ?
C6 Fe1 C7 96.59(18) . . ?
C5 Fe1 Se1 103.87(12) . . ?
C6 Fe1 Se1 99.28(13) . . ?
C7 Fe1 Se1 149.15(11) . . ?
C5 Fe1 Co1 153.23(13) . . ?
C6 Fe1 Co1 103.86(13) . . ?
C7 Fe1 Co1 94.29(11) . . ?
Se1 Fe1 Co1 56.258(19) . . ?
C5 Fe1 Co2 95.83(14) . . ?
C6 Fe1 Co2 154.37(13) . . ?
C7 Fe1 Co2 103.08(12) . . ?
Se1 Fe1 Co2 55.89(2) . . ?
Co1 Fe1 Co2 58.82(4) . . ?
C1 Co1 C2 98.24(15) . . ?
C1 Co1 N1 103.13(14) . . ?
C2 Co1 N1 102.67(13) . . ?
C1 Co1 Se1 102.30(11) . . ?
C2 Co1 Se1 146.83(10) . . ?
N1 Co1 Se1 97.71(8) . . ?
C1 Co1 Co2 151.84(11) . . ?
C2 Co1 Co2 94.35(10) . . ?
N1 Co1 Co2 98.49(7) . . ?
Se1 Co1 Co2 56.61(3) . . ?
C1 Co1 Fe1 92.55(12) . . ?
C2 Co1 Fe1 97.48(11) . . ?
N1 Co1 Fe1 152.24(7) . . ?
Se1 Co1 Fe1 56.13(3) . . ?
Co2 Co1 Fe1 60.77(4) . . ?
C4 Co2 C3 103.17(18) . . ?
C4 Co2 P1 105.37(13) . . ?
C3 Co2 P1 99.88(12) . . ?
C4 Co2 Se1 96.47(14) . . ?
C3 Co2 Se1 140.88(11) . . ?
P1 Co2 Se1 107.10(6) . . ?
C4 Co2 Co1 153.39(13) . . ?
C3 Co2 Co1 99.56(11) . . ?
P1 Co2 Co1 83.96(4) . . ?
Se1 Co2 Co1 56.93(3) . . ?
C4 Co2 Fe1 107.59(13) . . ?
C3 Co2 Fe1 85.61(11) . . ?
P1 Co2 Fe1 144.34(4) . . ?
Se1 Co2 Fe1 56.08(3) . . ?
Co1 Co2 Fe1 60.41(3) . . ?
Co2 Se1 Fe1 68.03(3) . . ?
Co2 Se1 Co1 66.46(5) . . ?
Fe1 Se1 Co1 67.61(3) . . ?
C13 P1 C19 103.64(15) . . ?
C13 P1 C8 101.10(14) . . ?
C19 P1 C8 102.79(14) . . ?
C13 P1 Co2 120.76(11) . . ?
C19 P1 Co2 113.00(11) . . ?
C8 P1 Co2 113.39(10) . . ?
C8 N1 C12 116.8(3) . . ?
C8 N1 Co1 121.00(19) . . ?
C12 N1 Co1 122.0(2) . . ?
O1 C1 Co1 177.7(3) . . ?
O2 C2 Co1 176.5(3) . . ?
O3 C3 Co2 177.8(3) . . ?
O4 C4 Co2 177.2(4) . . ?
O5 C5 Fe1 178.3(4) . . ?
O6 C6 Fe1 178.7(4) . . ?
O7 C7 Fe1 177.5(3) . . ?
N1 C8 C9 122.0(3) . . ?
N1 C8 P1 114.4(2) . . ?
C9 C8 P1 123.7(2) . . ?
C8 C9 C10 120.1(3) . . ?
C11 C10 C9 118.0(3) . . ?
C10 C11 C12 120.3(3) . . ?
N1 C12 C11 122.8(3) . . ?
C17 C13 C14 118.8(3) . . ?
C17 C13 P1 118.5(2) . . ?
C14 C13 P1 122.6(3) . . ?
C15 C14 C13 120.1(4) . . ?
C16 C15 C14 120.5(4) . . ?
C15 C16 C18 119.9(4) . . ?
C13 C17 C18 120.5(3) . . ?
C16 C18 C17 120.2(4) . . ?
C20 C19 C24 118.7(3) . . ?
C20 C19 P1 123.1(3) . . ?
C24 C19 P1 118.1(3) . . ?
C19 C20 C21 119.7(4) . . ?
C22 C21 C20 120.8(4) . . ?
C21 C22 C23 120.0(4) . . ?
C22 C23 C24 120.5(4) . . ?
C23 C24 C19 120.2(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
Fe1 C5 1.776(4) . ?
Fe1 C6 1.778(4) . ?
Fe1 C7 1.791(4) . ?
Fe1 Se1 2.2962(7) . ?
Fe1 Co1 2.5571(13) . ?
Fe1 Co2 2.5661(14) . ?
Co1 C1 1.769(3) . ?
Co1 C2 1.791(3) . ?
Co1 N1 2.024(2) . ?
Co1 Se1 2.2997(11) . ?
Co1 Co2 2.5157(10) . ?
Co2 C4 1.778(4) . ?
Co2 C3 1.783(4) . ?
Co2 P1 2.2045(16) . ?
Co2 Se1 2.2912(11) . ?
P1 C13 1.830(3) . ?
P1 C19 1.834(3) . ?
P1 C8 1.844(3) . ?
O1 C1 1.141(4) . ?
O2 C2 1.133(4) . ?
O3 C3 1.141(4) . ?
O4 C4 1.141(4) . ?
O5 C5 1.146(4) . ?
O6 C6 1.146(4) . ?
O7 C7 1.145(4) . ?
N1 C8 1.356(4) . ?
N1 C12 1.349(4) . ?
C8 C9 1.383(4) . ?
C9 C10 1.374(5) . ?
C10 C11 1.360(5) . ?
C11 C12 1.372(5) . ?
C13 C17 1.377(5) . ?
C13 C14 1.398(4) . ?
C14 C15 1.385(5) . ?
C15 C16 1.371(5) . ?
C16 C18 1.369(5) . ?
C17 C18 1.395(5) . ?
C19 C20 1.396(4) . ?
C19 C24 1.397(4) . ?
C20 C21 1.393(5) . ?
C21 C22 1.357(6) . ?
C22 C23 1.379(6) . ?
C23 C24 1.376(5) . ?
