#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:35:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179147 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310868.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_4310868
loop_
_publ_author_name
'Richard D. Adams'
'Shaobin Miao'
'Mark D. Smith'
'Horatio Farach'
'Charles Edwin Webster'
'Josiah Manson'
'Michael B. Hall'
_publ_section_title
;
 Nickel-Manganese Sulfido Carbonyl Cluster Complexes. Synthesis,
 Structure, and Properties of the Unusual Paramagnetic Complexes
 Cp2Ni2Mn(CO)3(μ3-E)2, E = S, Se
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2515
_journal_page_last               2525
_journal_paper_doi               10.1021/ic0354419
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C13 H10 Mn Ni2 O3 S2'
_chemical_formula_weight         450.69
_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                 99.6840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9856(4)
_cell_length_b                   10.5400(5)
_cell_length_c                   18.1775(8)
_cell_measurement_reflns_used    6147
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.24
_cell_volume                     1508.17(12)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11276
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    3.574
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0233
_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)+(0.0316P)²+0.0898P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                3404
_reflns_number_total             3750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354419si20031216_105958.cif
_cod_data_source_block           miaoii3s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310868
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.32439(3) 0.456819(18) 0.105184(11) 0.03271(7) Uani 1 1 d . . .
Ni2 Ni 0.28843(3) 0.755753(18) 0.111742(10) 0.03083(7) Uani 1 1 d . . .
Mn1 Mn 0.12873(3) 0.58704(2) 0.177653(13) 0.03103(7) Uani 1 1 d . . .
S1 S 0.14730(5) 0.59948(3) 0.05368(2) 0.03260(9) Uani 1 1 d . . .
S2 S 0.41846(5) 0.60806(4) 0.18142(2) 0.03386(10) Uani 1 1 d . . .
O20 O -0.0957(2) 0.36525(17) 0.16581(11) 0.0792(5) Uani 1 1 d . . .
O21 O 0.1868(2) 0.57437(15) 0.34209(8) 0.0654(4) Uani 1 1 d . . .
O22 O -0.1571(2) 0.76308(17) 0.17536(11) 0.0775(5) Uani 1 1 d . . .
C1 C 0.2346(4) 0.2772(2) 0.0654(2) 0.0810(10) Uani 1 1 d . . .
C2 C 0.3231(3) 0.26045(18) 0.13743(16) 0.0618(6) Uani 1 1 d . . .
C3 C 0.4879(3) 0.30347(19) 0.13872(12) 0.0521(5) Uani 1 1 d . . .
C4 C 0.5066(4) 0.3405(2) 0.06698(14) 0.0650(6) Uani 1 1 d . . .
C5 C 0.3505(5) 0.3277(3) 0.02203(14) 0.0852(11) Uani 1 1 d . . .
C6 C 0.2460(4) 0.94015(19) 0.15454(14) 0.0643(7) Uani 1 1 d . . .
C7 C 0.1549(4) 0.9269(2) 0.08393(17) 0.0667(7) Uani 1 1 d . . .
C8 C 0.2754(5) 0.9040(2) 0.03513(13) 0.0706(9) Uani 1 1 d . . .
C9 C 0.4361(4) 0.90417(18) 0.07769(15) 0.0599(6) Uani 1 1 d . . .
C10 C 0.4169(4) 0.9218(2) 0.15177(14) 0.0605(6) Uani 1 1 d . . .
C20 C -0.0083(3) 0.45235(19) 0.17099(11) 0.0476(4) Uani 1 1 d . . .
C21 C 0.1658(3) 0.57986(18) 0.27826(10) 0.0428(4) Uani 1 1 d . . .
C22 C -0.0451(3) 0.69451(19) 0.17672(10) 0.0471(4) Uani 1 1 d . . .
H1 H 0.119(5) 0.267(3) 0.0489(18) 0.114(12) Uiso 1 1 d . . .
H2 H 0.266(4) 0.232(3) 0.1792(15) 0.092(10) Uiso 1 1 d . . .
H3 H 0.570(3) 0.308(2) 0.1786(13) 0.073(7) Uiso 1 1 d . . .
H4 H 0.594(4) 0.367(3) 0.0563(16) 0.083(10) Uiso 1 1 d . . .
H5 H 0.326(4) 0.344(3) -0.0205(17) 0.091(10) Uiso 1 1 d . . .
H6 H 0.196(3) 0.952(3) 0.1956(15) 0.083(9) Uiso 1 1 d . . .
H7 H 0.031(4) 0.925(2) 0.0702(15) 0.083(9) Uiso 1 1 d . . .
H8 H 0.259(4) 0.889(2) -0.0041(16) 0.083(10) Uiso 1 1 d . . .
H9 H 0.535(3) 0.889(2) 0.0652(14) 0.058(7) Uiso 1 1 d . . .
H10 H 0.502(4) 0.921(3) 0.1922(16) 0.091(10) Uiso 1 1 d . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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 Ni1 C3 64.70(10) . . ?
C5 Ni1 C4 38.48(12) . . ?
C3 Ni1 C4 38.64(9) . . ?
C5 Ni1 C1 39.60(13) . . ?
C3 Ni1 C1 64.43(10) . . ?
C4 Ni1 C1 65.06(12) . . ?
C5 Ni1 C2 64.68(12) . . ?
C3 Ni1 C2 38.08(9) . . ?
C4 Ni1 C2 64.23(11) . . ?
C1 Ni1 C2 38.10(11) . . ?
C5 Ni1 S2 152.35(12) . . ?
C3 Ni1 S2 104.42(6) . . ?
C4 Ni1 S2 117.10(9) . . ?
C1 Ni1 S2 160.59(11) . . ?
C2 Ni1 S2 123.48(8) . . ?
C5 Ni1 S1 106.21(8) . . ?
C3 Ni1 S1 170.88(6) . . ?
C4 Ni1 S1 134.27(7) . . ?
C1 Ni1 S1 108.37(8) . . ?
C2 Ni1 S1 138.83(7) . . ?
S2 Ni1 S1 84.056(16) . . ?
C5 Ni1 Mn1 149.34(11) . . ?
C3 Ni1 Mn1 131.00(6) . . ?
C4 Ni1 Mn1 168.97(7) . . ?
C1 Ni1 Mn1 116.70(10) . . ?
C2 Ni1 Mn1 109.82(8) . . ?
S2 Ni1 Mn1 57.277(14) . . ?
S1 Ni1 Mn1 56.491(13) . . ?
C8 Ni2 C10 64.69(10) . . ?
C8 Ni2 C7 39.95(12) . . ?
C10 Ni2 C7 64.40(11) . . ?
C8 Ni2 C9 38.46(12) . . ?
C10 Ni2 C9 38.65(10) . . ?
C7 Ni2 C9 65.29(11) . . ?
C8 Ni2 C6 64.47(10) . . ?
C10 Ni2 C6 38.21(11) . . ?
C7 Ni2 C6 37.61(10) . . ?
C9 Ni2 C6 64.21(10) . . ?
C8 Ni2 S2 153.84(11) . . ?
C10 Ni2 S2 103.85(7) . . ?
C7 Ni2 S2 158.31(9) . . ?
C9 Ni2 S2 117.93(8) . . ?
C6 Ni2 S2 122.07(7) . . ?
C8 Ni2 S1 106.32(8) . . ?
C10 Ni2 S1 170.99(7) . . ?
C7 Ni2 S1 109.40(8) . . ?
C9 Ni2 S1 133.63(7) . . ?
C6 Ni2 S1 139.96(8) . . ?
S2 Ni2 S1 84.096(16) . . ?
C8 Ni2 Mn1 148.08(10) . . ?
C10 Ni2 Mn1 131.41(7) . . ?
C7 Ni2 Mn1 115.34(8) . . ?
C9 Ni2 Mn1 169.71(8) . . ?
C6 Ni2 Mn1 109.51(7) . . ?
S2 Ni2 Mn1 57.353(13) . . ?
S1 Ni2 Mn1 56.531(13) . . ?
C20 Mn1 C22 92.13(10) . . ?
C20 Mn1 C21 91.69(9) . . ?
C22 Mn1 C21 91.76(9) . . ?
C20 Mn1 S1 96.86(6) . . ?
C22 Mn1 S1 97.65(6) . . ?
C21 Mn1 S1 167.01(7) . . ?
C20 Mn1 S2 132.62(7) . . ?
C22 Mn1 S2 135.22(7) . . ?
C21 Mn1 S2 88.93(6) . . ?
S1 Mn1 S2 78.080(17) . . ?
C20 Mn1 Ni2 149.00(6) . . ?
C22 Mn1 Ni2 90.14(6) . . ?
C21 Mn1 Ni2 119.15(6) . . ?
S1 Mn1 Ni2 52.235(11) . . ?
S2 Mn1 Ni2 51.802(11) . . ?
C20 Mn1 Ni1 87.68(7) . . ?
C22 Mn1 Ni1 149.44(6) . . ?
C21 Mn1 Ni1 118.79(6) . . ?
S1 Mn1 Ni1 52.163(12) . . ?
S2 Mn1 Ni1 51.835(12) . . ?
Ni2 Mn1 Ni1 75.160(10) . . ?
Ni1 S1 Ni2 93.949(17) . . ?
Ni1 S1 Mn1 71.345(14) . . ?
Ni2 S1 Mn1 71.234(14) . . ?
Ni2 S2 Ni1 94.276(17) . . ?
Ni2 S2 Mn1 70.845(14) . . ?
Ni1 S2 Mn1 70.887(14) . . ?
C2 C1 C5 107.2(3) . . ?
C2 C1 Ni1 72.61(12) . . ?
C5 C1 Ni1 68.73(14) . . ?
C3 C2 C1 107.7(3) . . ?
C3 C2 Ni1 69.05(12) . . ?
C1 C2 Ni1 69.29(13) . . ?
C2 C3 C4 109.0(2) . . ?
C2 C3 Ni1 72.87(12) . . ?
C4 C3 Ni1 70.87(13) . . ?
C5 C4 C3 107.4(3) . . ?
C5 C4 Ni1 69.29(14) . . ?
C3 C4 Ni1 70.49(12) . . ?
C4 C5 C1 108.5(2) . . ?
C4 C5 Ni1 72.23(14) . . ?
C1 C5 Ni1 71.67(14) . . ?
C7 C6 C10 108.8(2) . . ?
C7 C6 Ni2 70.07(13) . . ?
C10 C6 Ni2 69.11(12) . . ?
C6 C7 C8 106.9(3) . . ?
C6 C7 Ni2 72.32(13) . . ?
C8 C7 Ni2 68.94(13) . . ?
C9 C8 C7 108.0(2) . . ?
C9 C8 Ni2 71.91(12) . . ?
C7 C8 Ni2 71.10(12) . . ?
C8 C9 C10 107.3(3) . . ?
C8 C9 Ni2 69.63(13) . . ?
C10 C9 Ni2 69.99(12) . . ?
C6 C10 C9 108.8(2) . . ?
C6 C10 Ni2 72.68(13) . . ?
C9 C10 Ni2 71.36(12) . . ?
O20 C20 Mn1 179.05(19) . . ?
O21 C21 Mn1 178.90(19) . . ?
O22 C22 Mn1 179.3(2) . . ?
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
Ni1 C5 2.070(2) . ?
Ni1 C3 2.1028(19) . ?
Ni1 C4 2.108(2) . ?
Ni1 C1 2.109(2) . ?
Ni1 C2 2.152(2) . ?
Ni1 S2 2.1623(4) . ?
Ni1 S1 2.1661(4) . ?
Ni1 Mn1 2.5986(3) . ?
Ni2 C8 2.084(2) . ?
Ni2 C10 2.096(2) . ?
Ni2 C7 2.113(2) . ?
Ni2 C9 2.113(2) . ?
Ni2 C6 2.142(2) . ?
Ni2 S2 2.1595(4) . ?
Ni2 S1 2.1672(4) . ?
Ni2 Mn1 2.5958(3) . ?
Mn1 C20 1.7841(19) . ?
Mn1 C22 1.789(2) . ?
Mn1 C21 1.8044(18) . ?
Mn1 S1 2.2869(5) . ?
Mn1 S2 2.3138(5) . ?
O20 C20 1.147(2) . ?
O21 C21 1.145(2) . ?
O22 C22 1.147(2) . ?
C1 C2 1.391(4) . ?
C1 C5 1.416(5) . ?
C2 C3 1.389(3) . ?
C3 C4 1.393(3) . ?
C4 C5 1.377(4) . ?
C6 C7 1.372(4) . ?
C6 C10 1.387(4) . ?
C7 C8 1.434(4) . ?
C8 C9 1.383(4) . ?
C9 C10 1.393(4) . ?
