#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:49:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179308 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/05/4320516.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_4320516
loop_
_publ_author_name
'Jaehong Han'
'Markos Koutmos'
'Saleem Al Ahmad'
'Dimitri Coucouvanis'
_publ_contact_author             'Dimitri Coucouvanis'
_publ_contact_author_address
;
  Dimitri Coucouvanis
  Department of Chemistry
  The University of Michigan
  Ann Arbor, MI 48109
  USA
;
_publ_contact_author_email       dcouc@umich.edu
_publ_section_title
;
 Rational Synthesis of High Nuclearity Mo/Fe/S Clusters: The Reductive
 Coupling Approach in the Convenient Synthesis of (Cl4-cat)2Mo2Fe6S8(PR3)6
 [R = Et, nPr, nBu] and the New
 [(Cl4-cat)2Mo2Fe2S3O(PEt3)3Cl].1/2(Fe(PEt3)2(MeCN)4) and
 (Cl4-cat)2Mo2Fe3S5(PEt3)5 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5985
_journal_page_last               5999
_journal_paper_doi               10.1021/ic0104914
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C68 H82 B2 Fe N4 P2'
_chemical_formula_weight         1094.79
_chemical_name_common            (BPh4)[Fe(PEt3)2(MeCN)4]
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.2090(10)
_cell_angle_beta                 114.5760(10)
_cell_angle_gamma                116.6450(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0756(10)
_cell_length_b                   12.2070(10)
_cell_length_c                   13.4024(11)
_cell_measurement_temperature    158(2)
_cell_volume                     1532.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15692
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  26.41
_exptl_absorpt_correction_T_min  1.75
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0388
_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)+(0.0503P)²+0.4966P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                5010
_reflns_number_total             6225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104914_6.cif
_cod_data_source_block           compound_IX
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Fe1 Fe 0.0000 0.0000 0.0000 0.01597(10) Uani 1 2 d S . .
P1 P 0.16082(5) 0.11157(4) 0.19253(4) 0.01839(12) Uani 1 1 d . . .
N1 N -0.15514(16) -0.02676(13) 0.02332(13) 0.0186(3) Uani 1 1 d . . .
N2 N -0.01527(15) -0.15634(14) 0.03152(13) 0.0194(3) Uani 1 1 d . . .
B1 B -0.4929(2) -0.75636(19) -0.25926(19) 0.0204(4) Uani 1 1 d . . .
C1 C -0.2479(2) -0.03678(16) 0.03426(16) 0.0205(4) Uani 1 1 d . . .
C2 C -0.3658(2) -0.0492(2) 0.0478(2) 0.0347(5) Uani 1 1 d . . .
H2A H -0.3478 -0.0540 0.1253 0.042 Uiso 1 1 calc R . .
H2B H -0.4541 -0.1275 -0.0091 0.042 Uiso 1 1 calc R . .
H2C H -0.3750 0.0255 0.0363 0.042 Uiso 1 1 calc R . .
C3 C -0.02201(19) -0.25044(17) 0.04562(17) 0.0223(4) Uani 1 1 d . . .
C4 C -0.0332(2) -0.37140(19) 0.0616(2) 0.0360(5) Uani 1 1 d . . .
H4A H -0.0378 -0.3810 0.1321 0.043 Uiso 1 1 calc R . .
H4B H 0.0504 -0.3717 0.0677 0.043 Uiso 1 1 calc R . .
H4C H -0.1197 -0.4428 -0.0043 0.043 Uiso 1 1 calc R . .
C5 C 0.0866(2) 0.09579(18) 0.28899(17) 0.0263(4) Uani 1 1 d . . .
H5A H 0.1637 0.1558 0.3664 0.032 Uiso 1 1 calc R . .
H5B H 0.0145 0.1214 0.2609 0.032 Uiso 1 1 calc R . .
C6 C 0.0172(2) -0.0399(2) 0.29896(19) 0.0336(5) Uani 1 1 d . . .
H6A H -0.0203 -0.0416 0.3516 0.040 Uiso 1 1 calc R . .
H6B H 0.0883 -0.0653 0.3287 0.040 Uiso 1 1 calc R . .
H6C H -0.0610 -0.0999 0.2230 0.040 Uiso 1 1 calc R . .
C7 C 0.2941(2) 0.06606(18) 0.25499(17) 0.0241(4) Uani 1 1 d . . .
H7A H 0.2442 -0.0267 0.2474 0.029 Uiso 1 1 calc R . .
H7B H 0.3431 0.0787 0.2093 0.029 Uiso 1 1 calc R . .
C8 C 0.4071(2) 0.1390(2) 0.38121(18) 0.0332(5) Uani 1 1 d . . .
H8A H 0.4732 0.1078 0.4063 0.040 Uiso 1 1 calc R . .
H8B H 0.3607 0.1252 0.4282 0.040 Uiso 1 1 calc R . .
H8C H 0.4598 0.2310 0.3900 0.040 Uiso 1 1 calc R . .
C9 C 0.2670(2) 0.28604(17) 0.22474(17) 0.0263(4) Uani 1 1 d . . .
H9A H 0.2014 0.3186 0.1955 0.032 Uiso 1 1 calc R . .
H9B H 0.3251 0.3248 0.3092 0.032 Uiso 1 1 calc R . .
C10 C 0.3662(2) 0.33112(18) 0.17363(19) 0.0321(5) Uani 1 1 d . . .
H10A H 0.4187 0.4251 0.1947 0.039 Uiso 1 1 calc R . .
H10B H 0.3097 0.2954 0.0897 0.039 Uiso 1 1 calc R . .
H10C H 0.4337 0.3018 0.2037 0.039 Uiso 1 1 calc R . .
C11 C -0.40738(19) -0.70178(16) -0.11607(16) 0.0218(4) Uani 1 1 d . . .
C12 C -0.4298(2) -0.62739(17) -0.05107(17) 0.0256(4) Uani 1 1 d . . .
H12A H -0.4951 -0.6012 -0.0907 0.031 Uiso 1 1 calc R . .
C13 C -0.3604(2) -0.59035(19) 0.06899(18) 0.0315(5) Uani 1 1 d . . .
H13A H -0.3799 -0.5408 0.1088 0.038 Uiso 1 1 calc R . .
C14 C -0.2636(2) -0.62531(19) 0.13030(18) 0.0332(5) Uani 1 1 d . . .
H14A H -0.2182 -0.6024 0.2118 0.040 Uiso 1 1 calc R . .
C15 C -0.2342(2) -0.69453(18) 0.07021(18) 0.0312(5) Uani 1 1 d . . .
H15A H -0.1664 -0.7178 0.1108 0.037 Uiso 1 1 calc R . .
C16 C -0.3034(2) -0.73010(17) -0.04919(17) 0.0256(4) Uani 1 1 d . . .
H16A H -0.2793 -0.7759 -0.0878 0.031 Uiso 1 1 calc R . .
C17 C -0.36822(19) -0.71960(17) -0.29483(16) 0.0205(4) Uani 1 1 d . . .
C18 C -0.2648(2) -0.58946(18) -0.26707(17) 0.0262(4) Uani 1 1 d . . .
H18A H -0.2660 -0.5259 -0.2241 0.031 Uiso 1 1 calc R . .
C19 C -0.1614(2) -0.5501(2) -0.29963(19) 0.0325(5) Uani 1 1 d . . .
H19A H -0.0955 -0.4612 -0.2807 0.039 Uiso 1 1 calc R . .
C20 C -0.1541(2) -0.6410(2) -0.36015(19) 0.0350(5) Uani 1 1 d . . .
H20A H -0.0834 -0.6148 -0.3827 0.042 Uiso 1 1 calc R . .
C21 C -0.2519(2) -0.7704(2) -0.38695(18) 0.0312(5) Uani 1 1 d . . .
H21A H -0.2478 -0.8337 -0.4274 0.037 Uiso 1 1 calc R . .
C22 C -0.3558(2) -0.80736(18) -0.35459(16) 0.0243(4) Uani 1 1 d . . .
H22A H -0.4216 -0.8964 -0.3740 0.029 Uiso 1 1 calc R . .
C23 C -0.58742(19) -0.69071(16) -0.31934(16) 0.0209(4) Uani 1 1 d . . .
C24 C -0.5753(2) -0.62755(17) -0.40239(16) 0.0240(4) Uani 1 1 d . . .
H24A H -0.5080 -0.6209 -0.4247 0.029 Uiso 1 1 calc R . .
C25 C -0.6578(2) -0.57432(18) -0.45319(18) 0.0297(5) Uani 1 1 d . . .
H25A H -0.6455 -0.5323 -0.5086 0.036 Uiso 1 1 calc R . .
C26 C -0.7572(2) -0.58217(19) -0.42364(18) 0.0326(5) Uani 1 1 d . . .
H26A H -0.8122 -0.5445 -0.4571 0.039 Uiso 1 1 calc R . .
C27 C -0.7755(2) -0.64613(19) -0.34424(18) 0.0303(5) Uani 1 1 d . . .
H27A H -0.8447 -0.6540 -0.3239 0.036 Uiso 1 1 calc R . .
C28 C -0.6923(2) -0.69884(17) -0.29445(17) 0.0247(4) Uani 1 1 d . . .
H28A H -0.7074 -0.7427 -0.2407 0.030 Uiso 1 1 calc R . .
C29 C -0.60392(19) -0.91482(16) -0.29973(16) 0.0212(4) Uani 1 1 d . . .
C30 C -0.7502(2) -0.97628(18) -0.37778(17) 0.0256(4) Uani 1 1 d . . .
H30A H -0.7870 -0.9260 -0.4133 0.031 Uiso 1 1 calc R . .
C31 C -0.8446(2) -1.10791(19) -0.40598(19) 0.0322(5) Uani 1 1 d . . .
H31A H -0.9433 -1.1443 -0.4577 0.039 Uiso 1 1 calc R . .
C32 C -0.7949(2) -1.18504(18) -0.35898(18) 0.0320(5) Uani 1 1 d . . .
H32A H -0.8588 -1.2742 -0.3766 0.038 Uiso 1 1 calc R . .
C33 C -0.6505(2) -1.13036(18) -0.28591(19) 0.0300(5) Uani 1 1 d . . .
H33A H -0.6139 -1.1826 -0.2552 0.036 Uiso 1 1 calc R . .
C34 C -0.5582(2) -0.99846(17) -0.25712(17) 0.0250(4) Uani 1 1 d . . .
H34A H -0.4596 -0.9633 -0.2061 0.030 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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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
N1 Fe1 N1 180.00(8) 2 . ?
N1 Fe1 N2 92.11(6) 2 2 ?
N1 Fe1 N2 87.89(6) . 2 ?
N1 Fe1 N2 87.89(6) 2 . ?
N1 Fe1 N2 92.11(6) . . ?
N2 Fe1 N2 180.00(17) 2 . ?
N1 Fe1 P1 90.86(5) 2 2 ?
N1 Fe1 P1 89.14(5) . 2 ?
N2 Fe1 P1 89.90(5) 2 2 ?
N2 Fe1 P1 90.10(5) . 2 ?
N1 Fe1 P1 89.14(5) 2 . ?
N1 Fe1 P1 90.86(5) . . ?
N2 Fe1 P1 90.10(5) 2 . ?
N2 Fe1 P1 89.90(5) . . ?
P1 Fe1 P1 180.00(3) 2 . ?
C7 P1 C5 104.60(9) . . ?
C7 P1 C9 103.80(9) . . ?
C5 P1 C9 102.27(9) . . ?
C7 P1 Fe1 112.90(6) . . ?
C5 P1 Fe1 116.59(7) . . ?
C9 P1 Fe1 115.17(7) . . ?
C1 N1 Fe1 175.73(14) . . ?
C3 N2 Fe1 175.95(15) . . ?
C17 B1 C23 110.85(15) . . ?
C17 B1 C29 111.71(15) . . ?
C23 B1 C29 108.22(15) . . ?
C17 B1 C11 105.76(14) . . ?
C23 B1 C11 111.73(15) . . ?
C29 B1 C11 108.57(14) . . ?
N1 C1 C2 179.8(2) . . ?
N2 C3 C4 178.9(2) . . ?
C6 C5 P1 113.73(14) . . ?
C8 C7 P1 115.85(13) . . ?
C10 C9 P1 114.69(13) . . ?
C12 C11 C16 114.05(18) . . ?
C12 C11 B1 125.63(17) . . ?
C16 C11 B1 120.32(16) . . ?
C13 C12 C11 123.01(19) . . ?
C14 C13 C12 120.5(2) . . ?
C13 C14 C15 118.5(2) . . ?
C14 C15 C16 120.36(19) . . ?
C15 C16 C11 123.44(19) . . ?
C22 C17 C18 114.94(17) . . ?
C22 C17 B1 125.63(16) . . ?
C18 C17 B1 119.41(16) . . ?
C19 C18 C17 123.00(19) . . ?
C18 C19 C20 120.02(19) . . ?
C21 C20 C19 118.86(19) . . ?
C20 C21 C22 120.0(2) . . ?
C21 C22 C17 123.15(18) . . ?
C28 C23 C24 114.40(17) . . ?
C28 C23 B1 121.72(16) . . ?
C24 C23 B1 123.83(16) . . ?
C25 C24 C23 122.78(18) . . ?
C26 C25 C24 120.56(19) . . ?
C25 C26 C27 118.80(19) . . ?
C26 C27 C28 119.90(19) . . ?
C27 C28 C23 123.53(18) . . ?
C30 C29 C34 114.09(17) . . ?
C30 C29 B1 123.36(16) . . ?
C34 C29 B1 122.56(17) . . ?
C31 C30 C29 123.27(19) . . ?
C32 C31 C30 120.2(2) . . ?
C31 C32 C33 118.82(18) . . ?
C32 C33 C34 120.09(19) . . ?
C33 C34 C29 123.37(19) . . ?
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 N1 1.9140(15) 2 ?
Fe1 N1 1.9140(15) . ?
Fe1 N2 1.9220(15) 2 ?
Fe1 N2 1.9220(15) . ?
Fe1 P1 2.3131(5) 2 ?
Fe1 P1 2.3131(5) . ?
P1 C7 1.8259(19) . ?
P1 C5 1.8302(19) . ?
P1 C9 1.8314(18) . ?
N1 C1 1.143(2) . ?
N2 C3 1.147(2) . ?
B1 C17 1.646(3) . ?
B1 C23 1.650(3) . ?
B1 C29 1.669(3) . ?
B1 C11 1.669(3) . ?
C1 C2 1.452(3) . ?
C3 C4 1.458(3) . ?
C5 C6 1.529(3) . ?
C7 C8 1.529(3) . ?
C9 C10 1.530(3) . ?
C11 C12 1.409(3) . ?
C11 C16 1.410(3) . ?
C12 C13 1.397(3) . ?
C13 C14 1.383(3) . ?
C14 C15 1.385(3) . ?
C15 C16 1.390(3) . ?
C17 C22 1.400(3) . ?
C17 C18 1.411(3) . ?
C18 C19 1.384(3) . ?
C19 C20 1.394(3) . ?
C20 C21 1.389(3) . ?
C21 C22 1.391(3) . ?
C23 C28 1.403(3) . ?
C23 C24 1.409(3) . ?
C24 C25 1.395(3) . ?
C25 C26 1.379(3) . ?
C26 C27 1.387(3) . ?
C27 C28 1.392(3) . ?
C29 C30 1.401(3) . ?
C29 C34 1.408(3) . ?
C30 C31 1.398(3) . ?
C31 C32 1.379(3) . ?
C32 C33 1.381(3) . ?
C33 C34 1.395(3) . ?
