#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:20:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179105 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/67/4306734.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_4306734
loop_
_publ_author_name
'Chia-Huei Lin'
'Chien-Ge Chen'
'Ming-Li Tsai'
'Gene-Hsiang Lee'
'Wen-Feng Liaw'
_publ_section_title
;
Monoanionic {Mn(NO)}5 and Dianionic {Mn(NO)}6 Thiolatonitrosylmanganese
Complexes: [(NO)Mn(L)2]- and [(NO)Mn(L)2]2- (LH2= 1,2-Benzenedithiol and
Toluene-3,4-dithiol)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11435
_journal_page_last               11443
_journal_paper_doi               10.1021/ic801553s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C84 H68 Mn N2 P4 S4'
_chemical_formula_weight         1412.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            8
_cell_length_a                   14.9431(3)
_cell_length_b                   27.2374(6)
_cell_length_c                   34.7540(8)
_cell_measurement_reflns_used    3855
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.34
_cell_volume                     14145.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART ApexCCD area detector'
_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  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            33975
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.8785
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            deep-yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0437
_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)+(0.0519P)²+32.5367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                3465
_reflns_number_total             4080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801553s_si_003.cif
_cod_data_source_block           ic9758
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4306734
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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
Mn Mn 0.6250 0.1250 0.1250 0.02549(16) Uani 1 4 d S . .
S1 S 0.74115(4) 0.08859(2) 0.085599(17) 0.03121(15) Uani 1 1 d . . .
C1 C 0.83883(13) 0.10880(7) 0.10902(6) 0.0216(4) Uani 1 1 d . . .
C2 C 0.92156(14) 0.09263(7) 0.09464(6) 0.0246(4) Uani 1 1 d . . .
H2A H 0.9221 0.0701 0.0738 0.029 Uiso 1 1 calc R . .
C3 C 1.00232(14) 0.10842(8) 0.10976(6) 0.0275(4) Uani 1 1 d . . .
H3A H 1.0572 0.0967 0.0994 0.033 Uiso 1 1 calc R . .
P1 P 0.63631(3) 0.430685(18) 0.082784(13) 0.01686(13) Uani 1 1 d . . .
N1 N 0.6250 0.45211(8) 0.1250 0.0202(5) Uani 1 2 d S . .
C4 C 0.53413(12) 0.43869(7) 0.05611(5) 0.0202(4) Uani 1 1 d . . .
C5 C 0.52744(14) 0.42384(9) 0.01766(6) 0.0309(5) Uani 1 1 d . . .
H5A H 0.5771 0.4091 0.0052 0.037 Uiso 1 1 calc R . .
C6 C 0.44806(15) 0.43084(10) -0.00197(6) 0.0368(6) Uani 1 1 d . . .
H6A H 0.4430 0.4205 -0.0280 0.044 Uiso 1 1 calc R . .
C7 C 0.37561(14) 0.45286(9) 0.01612(7) 0.0328(5) Uani 1 1 d . . .
H7A H 0.3212 0.4574 0.0025 0.039 Uiso 1 1 calc R . .
C8 C 0.38231(14) 0.46811(8) 0.05381(7) 0.0315(5) Uani 1 1 d . . .
H8A H 0.3329 0.4836 0.0660 0.038 Uiso 1 1 calc R . .
C9 C 0.46178(13) 0.46076(8) 0.07395(6) 0.0253(4) Uani 1 1 d . . .
H9A H 0.4663 0.4709 0.1000 0.030 Uiso 1 1 calc R . .
C10 C 0.66677(12) 0.36680(7) 0.08085(5) 0.0187(4) Uani 1 1 d . . .
C11 C 0.60350(13) 0.33016(7) 0.07465(5) 0.0215(4) Uani 1 1 d . . .
H11A H 0.5435 0.3387 0.0685 0.026 Uiso 1 1 calc R . .
C12 C 0.62797(14) 0.28124(8) 0.07747(6) 0.0266(4) Uani 1 1 d . . .
H12A H 0.5845 0.2563 0.0737 0.032 Uiso 1 1 calc R . .
C13 C 0.71592(15) 0.26864(8) 0.08572(6) 0.0283(5) Uani 1 1 d . . .
H13A H 0.7327 0.2351 0.0874 0.034 Uiso 1 1 calc R . .
C14 C 0.77915(14) 0.30502(8) 0.09148(6) 0.0293(5) Uani 1 1 d . . .
H14A H 0.8394 0.2964 0.0969 0.035 Uiso 1 1 calc R . .
C15 C 0.75490(13) 0.35382(8) 0.08941(6) 0.0249(4) Uani 1 1 d . . .
H15A H 0.7983 0.3787 0.0938 0.030 Uiso 1 1 calc R . .
C16 C 0.72405(12) 0.46364(7) 0.05846(5) 0.0191(4) Uani 1 1 d . . .
C17 C 0.76582(13) 0.44368(8) 0.02592(6) 0.0232(4) Uani 1 1 d . . .
H17A H 0.7475 0.4127 0.0162 0.028 Uiso 1 1 calc R . .
C18 C 0.83401(14) 0.46943(8) 0.00801(6) 0.0279(4) Uani 1 1 d . . .
H18A H 0.8627 0.4559 -0.0139 0.033 Uiso 1 1 calc R . .
C19 C 0.86057(14) 0.51473(8) 0.02185(6) 0.0278(5) Uani 1 1 d . . .
H19A H 0.9075 0.5321 0.0094 0.033 Uiso 1 1 calc R . .
C20 C 0.81888(14) 0.53499(8) 0.05396(6) 0.0258(4) Uani 1 1 d . . .
H20A H 0.8372 0.5662 0.0634 0.031 Uiso 1 1 calc R . .
C21 C 0.75056(13) 0.50960(7) 0.07215(6) 0.0223(4) Uani 1 1 d . . .
H21A H 0.7217 0.5235 0.0939 0.027 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'
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'
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'
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
S1 Mn S1 88.50(2) 8_544 . ?
S1 Mn S1 131.68(3) 8_544 14_545 ?
S1 Mn S1 111.18(3) . 14_545 ?
S1 Mn S1 111.18(3) 8_544 11_554 ?
S1 Mn S1 131.68(3) . 11_554 ?
S1 Mn S1 88.50(2) 14_545 11_554 ?
C1 S1 Mn 101.81(7) . . ?
C2 C1 C1 118.28(12) . 8_544 ?
C2 C1 S1 117.87(15) . . ?
C1 C1 S1 123.84(7) 8_544 . ?
C3 C2 C1 122.31(19) . . ?
C2 C3 C3 119.37(12) . 8_544 ?
N1 P1 C4 109.95(7) . . ?
N1 P1 C16 109.16(9) . . ?
C4 P1 C16 108.40(9) . . ?
N1 P1 C10 114.62(10) . . ?
C4 P1 C10 108.20(9) . . ?
C16 P1 C10 106.29(9) . . ?
P1 N1 P1 136.89(16) 11_554 . ?
C9 C4 C5 119.83(18) . . ?
C9 C4 P1 118.99(15) . . ?
C5 C4 P1 121.16(15) . . ?
C6 C5 C4 119.5(2) . . ?
C5 C6 C7 120.4(2) . . ?
C8 C7 C6 120.28(19) . . ?
C7 C8 C9 119.8(2) . . ?
C4 C9 C8 120.22(19) . . ?
C11 C10 C15 119.51(19) . . ?
C11 C10 P1 121.83(15) . . ?
C15 C10 P1 118.38(15) . . ?
C12 C11 C10 119.97(19) . . ?
C11 C12 C13 120.15(19) . . ?
C14 C13 C12 120.0(2) . . ?
C15 C14 C13 120.2(2) . . ?
C14 C15 C10 120.2(2) . . ?
C21 C16 C17 119.76(18) . . ?
C21 C16 P1 119.59(14) . . ?
C17 C16 P1 120.65(15) . . ?
C18 C17 C16 119.60(19) . . ?
C19 C18 C17 120.5(2) . . ?
C18 C19 C20 120.29(19) . . ?
C21 C20 C19 119.83(19) . . ?
C20 C21 C16 120.07(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
Mn S1 2.4230(5) 8_544 ?
Mn S1 2.4230(5) . ?
Mn S1 2.4230(5) 14_545 ?
Mn S1 2.4230(5) 11_554 ?
S1 C1 1.760(2) . ?
C1 C2 1.404(3) . ?
C1 C1 1.418(4) 8_544 ?
C2 C3 1.385(3) . ?
C3 C3 1.392(4) 8_544 ?
P1 N1 1.5880(10) . ?
P1 C4 1.7995(19) . ?
P1 C16 1.7999(19) . ?
P1 C10 1.800(2) . ?
N1 P1 1.5880(10) 11_554 ?
C4 C9 1.384(3) . ?
C4 C5 1.400(3) . ?
C5 C6 1.382(3) . ?
C6 C7 1.388(3) . ?
C7 C8 1.378(3) . ?
C8 C9 1.393(3) . ?
C10 C11 1.391(3) . ?
C10 C15 1.396(3) . ?
C11 C12 1.385(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.384(3) . ?
C14 C15 1.380(3) . ?
C16 C21 1.396(3) . ?
C16 C17 1.401(3) . ?
C17 C18 1.385(3) . ?
C18 C19 1.382(3) . ?
C19 C20 1.392(3) . ?
C20 C21 1.386(3) . ?
