#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:17:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178713 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/24/4082416.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_4082416
loop_
_publ_author_name
'Carroll, Maria E.'
'Chen, Jinzhu'
'Gray, Danielle E.'
'Lansing, James C.'
'Rauchfuss, Thomas B.'
'Schilter, David'
'Volkers, Phillip I.'
'Wilson, Scott R.'
_publ_section_title
;
 Ferrous Carbonyl Dithiolates as Precursors to FeFe, FeCo, and FeMn
 Carbonyl Dithiolates.
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              858
_journal_page_last               867
_journal_paper_doi               10.1021/om400752a
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C30 H26 Fe O2 P2 S2 '
_chemical_formula_sum            'C30 H26 Fe O2 P2 S2'
_chemical_formula_weight         600.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.678(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7098(15)
_cell_length_b                   9.2543(11)
_cell_length_c                   23.859(3)
_cell_measurement_temperature    193(2)
_cell_volume                     2737.9(6)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω 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  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24980
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_correction_T_min  0.8161
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0426
_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)+(0.0356P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                3989
_reflns_number_total             6723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400752a_si_003.cif
_cod_data_source_block           f89kfface
_cod_depositor_comments
'Adding full bibliography for 4082416--4082419.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4082416
loop_
_symmetry_equiv_pos_as_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_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
Fe1 Fe 0.33216(3) 0.06590(4) 0.114836(15) 0.02481(10) Uani 1 1 d .
S1 S 0.20744(6) -0.10510(7) 0.06949(3) 0.03343(17) Uani 1 1 d .
S2 S 0.29216(5) 0.00121(7) 0.20298(3) 0.02914(16) Uani 1 1 d .
P1 P 0.19840(5) 0.23059(7) 0.10910(3) 0.02384(16) Uani 1 1 d .
P2 P 0.43969(5) 0.24327(7) 0.15712(3) 0.02568(16) Uani 1 1 d .
O1 O 0.37068(16) 0.1143(2) 0.00005(8) 0.0485(6) Uani 1 1 d .
O2 O 0.49406(17) -0.1642(2) 0.14024(9) 0.0533(6) Uani 1 1 d .
C1 C 0.3560(2) 0.1002(3) 0.04538(12) 0.0318(6) Uani 1 1 d .
C2 C 0.4319(2) -0.0735(3) 0.13030(11) 0.0346(6) Uani 1 1 d .
C3 C 0.1988(2) -0.2173(3) 0.13042(11) 0.0405(7) Uani 1 1 d .
H3A H 0.1371 -0.2844 0.1191 0.049 Uiso 1 1 calc R
H3B H 0.2653 -0.2761 0.1412 0.049 Uiso 1 1 calc R
C4 C 0.1850(2) -0.1329(3) 0.18114(11) 0.0370(7) Uani 1 1 d .
H4A H 0.1850 -0.1998 0.2135 0.044 Uiso 1 1 calc R
H4B H 0.1144 -0.0832 0.1720 0.044 Uiso 1 1 calc R
C5 C 0.2521(2) 0.3772(2) 0.15766(10) 0.0248(6) Uani 1 1 d .
H5 H 0.2056 0.4494 0.1669 0.030 Uiso 1 1 calc R
C6 C 0.3562(2) 0.3816(3) 0.17971(10) 0.0277(6) Uani 1 1 d .
H6 H 0.3867 0.4544 0.2065 0.033 Uiso 1 1 calc R
C7 C 0.0721(2) 0.1888(2) 0.13059(10) 0.0247(6) Uani 1 1 d .
C8 C 0.0622(2) 0.2173(3) 0.18675(11) 0.0306(6) Uani 1 1 d .
H8 H 0.1212 0.2572 0.2138 0.037 Uiso 1 1 calc R
C9 C -0.0336(2) 0.1873(3) 0.20303(12) 0.0391(7) Uani 1 1 d .
H9 H -0.0398 0.2068 0.2413 0.047 Uiso 1 1 calc R
C10 C -0.1200(2) 0.1296(3) 0.16451(13) 0.0415(7) Uani 1 1 d .
H10 H -0.1856 0.1101 0.1760 0.050 Uiso 1 1 calc R
C11 C -0.1109(2) 0.0999(3) 0.10867(12) 0.0381(7) Uani 1 1 d .
H11 H -0.1701 0.0594 0.0819 0.046 Uiso 1 1 calc R
C12 C -0.0155(2) 0.1295(3) 0.09215(11) 0.0297(6) Uani 1 1 d .
H12 H -0.0097 0.1090 0.0539 0.036 Uiso 1 1 calc R
C13 C 0.15388(19) 0.3199(3) 0.03939(10) 0.0244(6) Uani 1 1 d .
C14 C 0.15316(19) 0.4693(3) 0.03413(11) 0.0288(6) Uani 1 1 d .
H14 H 0.1778 0.5273 0.0673 0.035 Uiso 1 1 calc R
C15 C 0.1170(2) 0.5349(3) -0.01888(12) 0.0350(7) Uani 1 1 d .
H15 H 0.1155 0.6373 -0.0218 0.042 Uiso 1 1 calc R
C16 C 0.0832(2) 0.4516(3) -0.06720(12) 0.0391(7) Uani 1 1 d .
H16 H 0.0576 0.4967 -0.1034 0.047 Uiso 1 1 calc R
C17 C 0.0865(2) 0.3028(3) -0.06333(11) 0.0396(7) Uani 1 1 d .
H17 H 0.0653 0.2455 -0.0970 0.048 Uiso 1 1 calc R
C18 C 0.1207(2) 0.2373(3) -0.01029(10) 0.0324(6) Uani 1 1 d .
H18 H 0.1216 0.1349 -0.0077 0.039 Uiso 1 1 calc R
C19 C 0.5504(2) 0.2122(3) 0.21951(10) 0.0289(6) Uani 1 1 d .
C20 C 0.5615(2) 0.0829(3) 0.25024(11) 0.0331(6) Uani 1 1 d .
H20 H 0.5085 0.0093 0.2403 0.040 Uiso 1 1 calc R
C21 C 0.6501(2) 0.0616(3) 0.29535(11) 0.0403(7) Uani 1 1 d .
H21 H 0.6572 -0.0267 0.3161 0.048 Uiso 1 1 calc R
C22 C 0.7273(2) 0.1664(3) 0.31025(12) 0.0430(7) Uani 1 1 d .
H22 H 0.7878 0.1500 0.3409 0.052 Uiso 1 1 calc R
C23 C 0.7173(2) 0.2956(3) 0.28085(12) 0.0464(8) Uani 1 1 d .
H23 H 0.7702 0.3690 0.2914 0.056 Uiso 1 1 calc R
C24 C 0.6293(2) 0.3177(3) 0.23565(12) 0.0403(7) Uani 1 1 d .
H24 H 0.6228 0.4066 0.2153 0.048 Uiso 1 1 calc R
C25 C 0.51100(19) 0.3438(3) 0.11107(10) 0.0275(6) Uani 1 1 d .
C26 C 0.4942(2) 0.4903(3) 0.09982(10) 0.0294(6) Uani 1 1 d .
H26 H 0.4407 0.5404 0.1144 0.035 Uiso 1 1 calc R
C27 C 0.5551(2) 0.5640(3) 0.06744(10) 0.0335(6) Uani 1 1 d .
H27 H 0.5438 0.6645 0.0604 0.040 Uiso 1 1 calc R
C28 C 0.6320(2) 0.4920(3) 0.04547(11) 0.0359(7) Uani 1 1 d .
H28 H 0.6739 0.5428 0.0235 0.043 Uiso 1 1 calc R
C29 C 0.6481(2) 0.3459(3) 0.05544(12) 0.0443(8) Uani 1 1 d .
H29 H 0.7007 0.2959 0.0401 0.053 Uiso 1 1 calc R
C30 C 0.5875(2) 0.2726(3) 0.08767(12) 0.0395(7) Uani 1 1 d .
H30 H 0.5983 0.1718 0.0940 0.047 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'
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'
S S 0.1246 0.1234 '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
C1 Fe1 C2 93.60(12)
C1 Fe1 P2 94.43(8)
C2 Fe1 P2 95.80(9)
C1 Fe1 P1 95.90(8)
C2 Fe1 P1 170.41(9)
P2 Fe1 P1 84.80(3)
C1 Fe1 S1 85.78(8)
C2 Fe1 S1 89.16(9)
P2 Fe1 S1 175.01(3)
P1 Fe1 S1 90.22(3)
C1 Fe1 S2 174.71(8)
C2 Fe1 S2 85.09(9)
P2 Fe1 S2 90.81(3)
P1 Fe1 S2 85.32(3)
S1 Fe1 S2 89.07(3)
C3 S1 Fe1 99.88(9)
C4 S2 Fe1 102.22(9)
C5 P1 C7 102.04(11)
C5 P1 C13 103.89(11)
C7 P1 C13 103.56(11)
C5 P1 Fe1 106.98(8)
C7 P1 Fe1 122.26(8)
C13 P1 Fe1 115.89(8)
C6 P2 C25 102.65(11)
C6 P2 C19 105.30(11)
C25 P2 C19 100.05(11)
C6 P2 Fe1 108.21(8)
C25 P2 Fe1 116.02(8)
C19 P2 Fe1 122.48(9)
O1 C1 Fe1 176.2(2)
O2 C2 Fe1 178.7(3)
C4 C3 S1 113.12(18)
C3 C4 S2 112.05(19)
C6 C5 P1 118.90(19)
C5 C6 P2 117.50(19)
C12 C7 C8 118.6(2)
C12 C7 P1 121.54(19)
C8 C7 P1 119.89(19)
C9 C8 C7 120.1(3)
C10 C9 C8 120.8(3)
C9 C10 C11 119.7(3)
C12 C11 C10 119.8(3)
C11 C12 C7 121.0(2)
C14 C13 C18 118.3(2)
C14 C13 P1 121.73(19)
C18 C13 P1 119.99(19)
C15 C14 C13 120.8(2)
C16 C15 C14 119.9(2)
C15 C16 C17 120.3(3)
C16 C17 C18 119.8(3)
C17 C18 C13 120.8(3)
C24 C19 C20 118.2(2)
C24 C19 P2 119.54(19)
C20 C19 P2 122.2(2)
C21 C20 C19 120.0(3)
C22 C21 C20 120.9(3)
C21 C22 C23 120.1(3)
C22 C23 C24 119.5(3)
C23 C24 C19 121.4(3)
C30 C25 C26 118.5(2)
C30 C25 P2 119.0(2)
C26 C25 P2 122.55(19)
C27 C26 C25 120.4(2)
C28 C27 C26 120.2(3)
C27 C28 C29 119.9(3)
C28 C29 C30 119.9(3)
C29 C30 C25 121.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 C1 1.777(3)
Fe1 C2 1.790(3)
Fe1 P2 2.2304(8)
Fe1 P1 2.2648(7)
Fe1 S1 2.3313(8)
Fe1 S2 2.3471(7)
S1 C3 1.809(3)
S2 C4 1.832(3)
P1 C5 1.817(2)
P1 C7 1.830(2)
P1 C13 1.832(2)
P2 C6 1.819(2)
P2 C25 1.825(2)
P2 C19 1.833(2)
O1 C1 1.144(3)
O2 C2 1.141(3)
C3 C4 1.482(3)
C5 C6 1.313(3)
C7 C12 1.391(3)
C7 C8 1.398(3)
C8 C9 1.385(3)
C9 C10 1.376(4)
C10 C11 1.390(4)
C11 C12 1.382(3)
C13 C14 1.388(3)
C13 C18 1.395(3)
C14 C15 1.387(3)
C15 C16 1.375(4)
C16 C17 1.380(4)
C17 C18 1.384(3)
C19 C24 1.391(3)
C19 C20 1.394(3)
C20 C21 1.390(4)
C21 C22 1.370(4)
C22 C23 1.377(4)
C23 C24 1.387(4)
C25 C30 1.389(3)
C25 C26 1.390(3)
C26 C27 1.387(3)
C27 C28 1.378(4)
C28 C29 1.380(4)
C29 C30 1.380(3)
