#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/24/4082419.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_4082419
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         'C34 H31 Co Fe O P2 S2 '
_chemical_formula_sum            'C34 H31 Co Fe O P2 S2'
_chemical_formula_weight         696.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   16.0226(10)
_cell_length_b                   21.7926(11)
_cell_length_c                   8.8475(6)
_cell_measurement_temperature    193(2)
_cell_volume                     3089.3(3)
_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  'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from 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  0.0882
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            19007
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.8420
_exptl_absorpt_correction_T_min  0.6301
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0352
_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)+(0.0501P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                3110
_reflns_number_total             3903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400752a_si_003.cif
_cod_data_source_block           ga55face
_cod_depositor_comments
'Adding full bibliography for 4082416--4082419.cif.'
_cod_original_sg_symbol_Hall     '-P 2ac 2n '
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4082419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Co1 Co 0.16010(2) 0.2500 0.97061(4) 0.02089(11) Uani 1 2 d S
Fe1 Fe 0.29958(2) 0.2500 0.84299(5) 0.01726(11) Uani 1 2 d S
P1 P 0.37269(3) 0.31906(2) 0.96780(6) 0.02037(13) Uani 1 1 d .
S4 S 0.19625(3) 0.31631(2) 0.79897(6) 0.02266(13) Uani 1 1 d .
O1 O 0.36889(15) 0.2500 0.5394(3) 0.0375(5) Uani 1 2 d S
C2 C 0.45027(12) 0.28035(8) 1.0836(3) 0.0266(4) Uani 1 1 d .
H2 H 0.4886 0.3024 1.1408 0.032 Uiso 1 1 calc R
C17 C 0.12469(14) 0.30252(9) 1.1528(3) 0.0293(5) Uani 1 1 d .
H17 H 0.1405 0.3431 1.1687 0.035 Uiso 1 1 calc R
C9 C 0.32140(13) 0.36982(8) 1.1049(3) 0.0248(4) Uani 1 1 d .
C1 C 0.34768(17) 0.2500 0.6649(4) 0.0227(6) Uani 1 2 d S
C3 C 0.43712(12) 0.37608(8) 0.8678(3) 0.0260(5) Uani 1 1 d .
C15 C 0.14703(14) 0.28475(9) 0.6282(3) 0.0336(5) Uani 1 1 d .
H15A H 0.0900 0.2994 0.6218 0.040 Uiso 1 1 calc R
H15B H 0.1768 0.2994 0.5398 0.040 Uiso 1 1 calc R
C18 C 0.05305(13) 0.28234(9) 1.0715(3) 0.0303(5) Uani 1 1 d .
H18 H 0.0133 0.3074 1.0264 0.036 Uiso 1 1 calc R
C10 C 0.27465(14) 0.41955(8) 1.0498(3) 0.0297(5) Uani 1 1 d .
H10 H 0.2732 0.4275 0.9465 0.036 Uiso 1 1 calc R
C8 C 0.49813(16) 0.40929(11) 0.9432(3) 0.0476(7) Uani 1 1 d .
H8 H 0.5051 0.4041 1.0468 0.057 Uiso 1 1 calc R
C14 C 0.32263(14) 0.35866(10) 1.2597(3) 0.0321(5) Uani 1 1 d .
H14 H 0.3535 0.3260 1.2978 0.039 Uiso 1 1 calc R
C16 C 0.16743(19) 0.2500 1.2050(4) 0.0299(7) Uani 1 2 d S
H16 H 0.2156 0.2500 1.2638 0.036 Uiso 1 2 calc SR
C13 C 0.27774(17) 0.39628(11) 1.3581(3) 0.0437(6) Uani 1 1 d .
H13 H 0.2788 0.3886 1.4615 0.052 Uiso 1 1 calc R
C11 C 0.23057(16) 0.45681(9) 1.1490(3) 0.0401(6) Uani 1 1 d .
H11 H 0.2002 0.4899 1.1119 0.048 Uiso 1 1 calc R
C6 C 0.53889(18) 0.45884(12) 0.7142(4) 0.0570(8) Uani 1 1 d .
H6 H 0.5737 0.4857 0.6624 0.068 Uiso 1 1 calc R
C5 C 0.4771(2) 0.42775(11) 0.6370(4) 0.0586(8) Uani 1 1 d .
H5 H 0.4691 0.4345 0.5342 0.070 Uiso 1 1 calc R
C12 C 0.23156(17) 0.44505(10) 1.3019(3) 0.0462(7) Uani 1 1 d .
H12 H 0.2012 0.4698 1.3676 0.055 Uiso 1 1 calc R
C4 C 0.42697(17) 0.38627(10) 0.7146(3) 0.0428(6) Uani 1 1 d .
H4 H 0.3858 0.3649 0.6624 0.051 Uiso 1 1 calc R
C7 C 0.54917(17) 0.45046(12) 0.8653(4) 0.0599(9) Uani 1 1 d .
H7 H 0.5903 0.4722 0.9168 0.072 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'
Co Co 0.3494 0.9721 '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
C17 Co1 C17 67.62(12) . 7_565
C17 Co1 C18 67.70(9) . 7_565
C17 Co1 C18 40.49(9) 7_565 7_565
C17 Co1 C18 40.49(9) . .
C17 Co1 C18 67.70(9) 7_565 .
C18 Co1 C18 40.05(11) 7_565 .
C17 Co1 C16 39.92(7) . .
C17 Co1 C16 39.92(8) 7_565 .
C18 Co1 C16 67.29(10) 7_565 .
C18 Co1 C16 67.29(10) . .
C17 Co1 S4 104.54(6) . .
C17 Co1 S4 172.08(6) 7_565 .
C18 Co1 S4 138.80(6) 7_565 .
C18 Co1 S4 107.30(6) . .
C16 Co1 S4 133.01(4) . .
C17 Co1 S4 172.08(6) . 7_565
C17 Co1 S4 104.54(6) 7_565 7_565
C18 Co1 S4 107.30(6) 7_565 7_565
C18 Co1 S4 138.80(7) . 7_565
C16 Co1 S4 133.01(4) . 7_565
S4 Co1 S4 83.28(3) . 7_565
C17 Co1 Fe1 126.85(6) . .
C17 Co1 Fe1 126.85(6) 7_565 .
C18 Co1 Fe1 159.97(6) 7_565 .
C18 Co1 Fe1 159.96(6) . .
C16 Co1 Fe1 113.56(8) . .
S4 Co1 Fe1 56.456(16) . .
S4 Co1 Fe1 56.457(16) 7_565 .
C1 Fe1 P1 102.51(7) . .
C1 Fe1 P1 102.51(7) . 7_565
P1 Fe1 P1 86.15(3) . 7_565
C1 Fe1 S4 99.74(7) . .
P1 Fe1 S4 92.267(19) . .
P1 Fe1 S4 157.51(3) 7_565 .
C1 Fe1 S4 99.74(7) . 7_565
P1 Fe1 S4 157.51(3) . 7_565
P1 Fe1 S4 92.266(19) 7_565 7_565
S4 Fe1 S4 80.71(3) . 7_565
C1 Fe1 Co1 142.87(9) . .
P1 Fe1 Co1 104.39(2) . .
P1 Fe1 Co1 104.39(2) 7_565 .
S4 Fe1 Co1 54.310(16) . .
S4 Fe1 Co1 54.311(16) 7_565 .
C2 P1 C9 102.32(10) . .
C2 P1 C3 101.57(9) . .
C9 P1 C3 99.31(9) . .
C2 P1 Fe1 109.20(6) . .
C9 P1 Fe1 120.31(7) . .
C3 P1 Fe1 121.19(8) . .
C15 S4 Co1 102.19(8) . .
C15 S4 Fe1 102.68(7) . .
Co1 S4 Fe1 69.234(19) . .
C2 C2 P1 117.64(6) 7_565 .
C16 C17 C18 107.81(19) . .
C16 C17 Co1 70.81(15) . .
C18 C17 Co1 69.80(12) . .
C14 C9 C10 119.0(2) . .
C14 C9 P1 122.59(16) . .
C10 C9 P1 118.32(17) . .
O1 C1 Fe1 171.0(3) . .
C4 C3 C8 118.1(2) . .
C4 C3 P1 120.89(16) . .
C8 C3 P1 121.04(19) . .
C15 C15 S4 111.97(7) 7_565 .
C18 C18 C17 107.99(12) 7_565 .
C18 C18 Co1 69.98(6) 7_565 .
C17 C18 Co1 69.70(12) . .
C11 C10 C9 120.2(2) . .
C3 C8 C7 120.7(3) . .
C9 C14 C13 120.3(2) . .
C17 C16 C17 108.4(3) . 7_565
C17 C16 Co1 69.26(16) . .
C17 C16 Co1 69.27(16) 7_565 .
C12 C13 C14 120.1(2) . .
C12 C11 C10 120.4(2) . .
C7 C6 C5 120.5(2) . .
C6 C5 C4 119.3(3) . .
C11 C12 C13 120.0(2) . .
C3 C4 C5 121.4(2) . .
C6 C7 C8 120.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C17 2.057(2) .
Co1 C17 2.057(2) 7_565
Co1 C18 2.058(2) 7_565
Co1 C18 2.058(2) .
Co1 C16 2.077(3) .
Co1 S4 2.1748(6) .
Co1 S4 2.1749(6) 7_565
Co1 Fe1 2.5038(5) .
Fe1 C1 1.754(3) .
Fe1 P1 2.2038(5) .
Fe1 P1 2.2038(5) 7_565
Fe1 S4 2.2318(5) .
Fe1 S4 2.2319(5) 7_565
P1 C2 1.819(2) .
P1 C9 1.836(2) .
P1 C3 1.842(2) .
S4 C15 1.838(2) .
O1 C1 1.161(4) .
C2 C2 1.323(4) 7_565
C17 C16 1.411(3) .
C17 C18 1.424(3) .
C9 C14 1.392(3) .
C9 C10 1.405(3) .
C3 C4 1.383(3) .
C3 C8 1.388(3) .
C15 C15 1.515(4) 7_565
C18 C18 1.409(4) 7_565
C10 C11 1.389(3) .
C8 C7 1.396(4) .
C14 C13 1.395(3) .
C16 C17 1.411(3) 7_565
C13 C12 1.387(4) .
C11 C12 1.377(4) .
C6 C7 1.359(4) .
C6 C5 1.380(4) .
C5 C4 1.391(4) .
