#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:52:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179159 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/20/4312022.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_4312022
loop_
_publ_author_name
'Anasuya Sanyal'
'Priyabrata Banerjee'
'Gene-Hsiang Lee'
'Shie-Ming Peng'
'Chen-Hsiung Hung'
'Sreebrata Goswami'
_publ_section_title
;
 Unusual Reduction of Ammonium Heptamolybdate to Novel
 Molybdenum(IV)-Stabilized Azo Anion Radical Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7456
_journal_page_last               7462
_journal_paper_doi               10.1021/ic049671e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C36 H30 Mo N8 S2'
_chemical_formula_weight         734.74
_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                107.781(1)
_cell_angle_beta                 105.807(1)
_cell_angle_gamma                98.666(1)
_cell_formula_units_Z            2
_cell_length_a                   10.5691(4)
_cell_length_b                   13.9169(6)
_cell_length_c                   14.5209(6)
_cell_measurement_reflns_used    4835
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.32
_cell_measurement_theta_min      2.27
_cell_volume                     1892.11(14)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25196
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.8995
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0601
_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)+(0.1006P)²+1.0656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                6789
_reflns_number_total             8664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049671esi20040730_064046.cif
_cod_data_source_block           ic10097
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_cell_volume        1892.11(13)
_cod_database_code               4312022
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
Mo1 Mo 0.70130(3) 0.84476(3) 0.66444(3) 0.04017(14) Uani 1 1 d . . .
S1 S 0.6275(2) 0.83470(18) 0.37008(16) 0.1030(6) Uani 1 1 d . . .
S2 S 0.88698(16) 0.87315(12) 0.97825(11) 0.0742(4) Uani 1 1 d . . .
N1 N 0.6255(4) 0.7396(3) 0.5207(3) 0.0546(10) Uani 1 1 d . . .
N2 N 0.4995(3) 0.8032(3) 0.6414(3) 0.0431(8) Uani 1 1 d . . .
N3 N 0.4390(4) 0.8472(3) 0.7079(3) 0.0515(9) Uani 1 1 d . . .
N4 N 0.6614(4) 0.9519(3) 0.7841(3) 0.0485(8) Uani 1 1 d . . .
N5 N 0.7553(4) 0.9745(3) 0.6261(3) 0.0483(8) Uani 1 1 d . . .
N6 N 0.9647(4) 0.9331(3) 0.6426(3) 0.0508(9) Uani 1 1 d . . .
N7 N 0.8989(3) 0.8664(3) 0.6755(3) 0.0422(8) Uani 1 1 d . . .
N8 N 0.7701(3) 0.7628(3) 0.7515(3) 0.0453(8) Uani 1 1 d . . .
C1 C 0.7046(5) 0.7000(4) 0.4573(4) 0.0626(13) Uani 1 1 d . . .
C2 C 0.7621(4) 0.6146(3) 0.4702(3) 0.0427(9) Uani 1 1 d . . .
H2A H 0.7471 0.5831 0.5156 0.051 Uiso 1 1 calc R . .
C3 C 0.8411(7) 0.5831(6) 0.4101(6) 0.096(2) Uani 1 1 d . . .
H3A H 0.8903 0.5352 0.4208 0.116 Uiso 1 1 calc R . .
C4 C 0.8472(8) 0.6236(7) 0.3327(6) 0.106(3) Uani 1 1 d . . .
H4A H 0.8960 0.5984 0.2902 0.128 Uiso 1 1 calc R . .
C5 C 0.7848(6) 0.6967(5) 0.3196(5) 0.0791(17) Uani 1 1 d . . .
H5A H 0.7889 0.7212 0.2674 0.095 Uiso 1 1 calc R . .
C6 C 0.7129(6) 0.7372(5) 0.3836(5) 0.0763(16) Uani 1 1 d . . .
C7 C 0.4881(4) 0.6875(4) 0.4848(4) 0.0503(10) Uani 1 1 d . . .
C8 C 0.4182(5) 0.6075(4) 0.3893(4) 0.0701(15) Uani 1 1 d . . .
H8A H 0.4626 0.5849 0.3427 0.084 Uiso 1 1 calc R . .
C9 C 0.2817(5) 0.5626(5) 0.3655(5) 0.0771(17) Uani 1 1 d . . .
H9A H 0.2340 0.5109 0.3013 0.093 Uiso 1 1 calc R . .
C10 C 0.2154(5) 0.5924(5) 0.4341(5) 0.0723(15) Uani 1 1 d . . .
H10A H 0.1253 0.5575 0.4175 0.087 Uiso 1 1 calc R . .
C11 C 0.2802(5) 0.6733(4) 0.5275(4) 0.0588(12) Uani 1 1 d . . .
H11A H 0.2338 0.6956 0.5727 0.071 Uiso 1 1 calc R . .
C12 C 0.4159(4) 0.7204(3) 0.5519(3) 0.0465(9) Uani 1 1 d . . .
C13 C 0.5296(5) 0.9283(4) 0.7850(4) 0.0516(11) Uani 1 1 d . . .
C14 C 0.4946(6) 0.9922(5) 0.8652(4) 0.0702(15) Uani 1 1 d . . .
H14A H 0.4070 0.9753 0.8671 0.084 Uiso 1 1 calc R . .
C15 C 0.5862(7) 1.0768(5) 0.9387(5) 0.0802(18) Uani 1 1 d . . .
H15A H 0.5623 1.1183 0.9915 0.096 Uiso 1 1 calc R . .
C16 C 0.7177(7) 1.1029(5) 0.9360(5) 0.0778(16) Uani 1 1 d . . .
H16A H 0.7815 1.1625 0.9859 0.093 Uiso 1 1 calc R . .
C17 C 0.7508(6) 1.0400(4) 0.8598(4) 0.0666(14) Uani 1 1 d . . .
H17A H 0.8388 1.0575 0.8588 0.080 Uiso 1 1 calc R . .
C18 C 0.6964(4) 0.7249(3) 0.8083(3) 0.0457(9) Uani 1 1 d . . .
C19 C 0.7360(5) 0.7718(4) 0.9135(4) 0.0568(11) Uani 1 1 d . . .
C20 C 0.6564(7) 0.7367(5) 0.9652(5) 0.0806(18) Uani 1 1 d . . .
H20A H 0.6822 0.7675 1.0363 0.097 Uiso 1 1 calc R . .
C21 C 0.5404(7) 0.6569(6) 0.9116(6) 0.091(2) Uani 1 1 d . . .
H21A H 0.4900 0.6326 0.9470 0.109 Uiso 1 1 calc R . .
C22 C 0.4978(6) 0.6124(5) 0.8062(5) 0.0765(16) Uani 1 1 d . . .
H22A H 0.4164 0.5611 0.7697 0.092 Uiso 1 1 calc R . .
C23 C 0.5764(4) 0.6449(3) 0.7571(4) 0.0514(10) Uani 1 1 d . . .
H23A H 0.5498 0.6127 0.6861 0.062 Uiso 1 1 calc R . .
C24 C 0.9012(4) 0.7487(3) 0.7604(3) 0.0442(9) Uani 1 1 d . . .
C25 C 0.9629(5) 0.6874(4) 0.8074(4) 0.0522(10) Uani 1 1 d . . .
H25A H 0.9179 0.6509 0.8381 0.063 Uiso 1 1 calc R . .
C26 C 1.0930(5) 0.6809(4) 0.8086(4) 0.0579(12) Uani 1 1 d . . .
H26A H 1.1340 0.6387 0.8395 0.070 Uiso 1 1 calc R . .
C27 C 1.1623(5) 0.7348(4) 0.7656(4) 0.0600(12) Uani 1 1 d . . .
H27A H 1.2494 0.7292 0.7674 0.072 Uiso 1 1 calc R . .
C28 C 1.1025(4) 0.7984(4) 0.7188(4) 0.0517(11) Uani 1 1 d . . .
H28A H 1.1492 0.8360 0.6899 0.062 Uiso 1 1 calc R . .
C29 C 0.9724(4) 0.8041(3) 0.7165(3) 0.0433(9) Uani 1 1 d . . .
C30 C 0.8832(5) 0.9920(4) 0.6174(4) 0.0530(11) Uani 1 1 d . . .
C31 C 0.9263(7) 1.0724(5) 0.5842(5) 0.0759(16) Uani 1 1 d . . .
H31A H 1.0110 1.0832 0.5762 0.091 Uiso 1 1 calc R . .
C32 C 0.8425(8) 1.1341(6) 0.5641(6) 0.096(2) Uani 1 1 d . . .
H32A H 0.8696 1.1870 0.5415 0.115 Uiso 1 1 calc R . .
C33 C 0.7153(7) 1.1180(5) 0.5772(6) 0.0874(19) Uani 1 1 d . . .
H33A H 0.6591 1.1617 0.5658 0.105 Uiso 1 1 calc R . .
C34 C 0.6753(6) 1.0395(4) 0.6064(4) 0.0668(14) Uani 1 1 d . . .
H34A H 0.5900 1.0287 0.6135 0.080 Uiso 1 1 calc R . .
C35 C 0.6667(15) 0.8660(13) 0.2725(10) 0.231(8) Uani 1 1 d . . .
H35A H 0.6236 0.9191 0.2603 0.346 Uiso 1 1 calc R . .
H35B H 0.6347 0.8049 0.2109 0.346 Uiso 1 1 calc R . .
H35C H 0.7635 0.8913 0.2924 0.346 Uiso 1 1 calc R . .
C36 C 0.8585(8) 0.9471(6) 1.0912(5) 0.115(3) Uani 1 1 d . . .
H36A H 0.9360 1.0052 1.1326 0.172 Uiso 1 1 calc R . .
H36B H 0.8448 0.9037 1.1296 0.172 Uiso 1 1 calc R . .
H36C H 0.7793 0.9723 1.0723 0.172 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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 Mo1 N8 104.34(16) . . ?
N1 Mo1 N7 96.62(14) . . ?
N8 Mo1 N7 77.33(14) . . ?
N1 Mo1 N2 77.08(14) . . ?
N8 Mo1 N2 100.00(14) . . ?
N7 Mo1 N2 172.44(13) . . ?
N1 Mo1 N5 96.72(16) . . ?
N8 Mo1 N5 144.43(15) . . ?
N7 Mo1 N5 71.97(14) . . ?
N2 Mo1 N5 112.59(14) . . ?
N1 Mo1 N4 146.62(16) . . ?
N8 Mo1 N4 92.92(14) . . ?
N7 Mo1 N4 115.15(14) . . ?
N2 Mo1 N4 71.86(14) . . ?
N5 Mo1 N4 84.38(14) . . ?
C35 S1 C6 104.3(5) . . ?
C19 S2 C36 102.7(3) . . ?
C7 N1 C1 116.5(4) . . ?
C7 N1 Mo1 117.1(3) . . ?
C1 N1 Mo1 125.6(3) . . ?
N3 N2 C12 116.4(3) . . ?
N3 N2 Mo1 125.0(3) . . ?
C12 N2 Mo1 118.6(3) . . ?
C13 N3 N2 109.0(3) . . ?
C17 N4 C13 117.7(4) . . ?
C17 N4 Mo1 127.1(3) . . ?
C13 N4 Mo1 115.2(3) . . ?
C34 N5 C30 118.7(4) . . ?
C34 N5 Mo1 126.2(3) . . ?
C30 N5 Mo1 115.1(3) . . ?
C30 N6 N7 107.8(3) . . ?
N6 N7 C29 117.4(3) . . ?
N6 N7 Mo1 125.1(3) . . ?
C29 N7 Mo1 117.5(3) . . ?
C24 N8 C18 119.7(4) . . ?
C24 N8 Mo1 116.7(3) . . ?
C18 N8 Mo1 123.5(3) . . ?
C6 C1 N1 119.3(5) . . ?
C6 C1 C2 122.2(5) . . ?
N1 C1 C2 118.3(4) . . ?
C3 C2 C1 115.4(5) . . ?
C2 C3 C4 120.5(7) . . ?
C5 C4 C3 121.2(6) . . ?
C4 C5 C6 120.5(7) . . ?
C1 C6 C5 119.6(6) . . ?
C1 C6 S1 117.7(5) . . ?
C5 C6 S1 122.7(5) . . ?
N1 C7 C8 125.8(4) . . ?
N1 C7 C12 115.7(4) . . ?
C8 C7 C12 118.5(4) . . ?
C9 C8 C7 118.8(5) . . ?
C10 C9 C8 121.6(5) . . ?
C9 C10 C11 121.0(5) . . ?
C10 C11 C12 118.2(5) . . ?
C11 C12 N2 127.3(4) . . ?
C11 C12 C7 121.8(4) . . ?
N2 C12 C7 110.9(4) . . ?
N3 C13 N4 118.4(4) . . ?
N3 C13 C14 122.0(5) . . ?
N4 C13 C14 119.5(5) . . ?
C15 C14 C13 120.6(5) . . ?
C14 C15 C16 120.0(5) . . ?
C17 C16 C15 118.9(6) . . ?
C16 C17 N4 123.2(5) . . ?
C19 C18 C23 118.5(4) . . ?
C19 C18 N8 120.8(4) . . ?
C23 C18 N8 120.5(4) . . ?
C18 C19 C20 119.0(5) . . ?
C18 C19 S2 118.6(4) . . ?
C20 C19 S2 122.5(4) . . ?
C21 C20 C19 120.4(6) . . ?
C20 C21 C22 120.9(6) . . ?
C23 C22 C21 118.4(6) . . ?
C22 C23 C18 122.8(5) . . ?
C25 C24 C29 119.1(4) . . ?
C25 C24 N8 126.4(4) . . ?
C29 C24 N8 114.5(4) . . ?
C24 C25 C26 119.3(5) . . ?
C27 C26 C25 121.6(5) . . ?
C26 C27 C28 120.1(4) . . ?
C29 C28 C27 118.5(4) . . ?
C28 C29 C24 121.5(4) . . ?
C28 C29 N7 125.9(4) . . ?
C24 C29 N7 112.5(3) . . ?
N6 C30 N5 119.0(4) . . ?
N6 C30 C31 121.0(5) . . ?
N5 C30 C31 120.0(5) . . ?
C32 C31 C30 119.2(6) . . ?
C31 C32 C33 120.0(6) . . ?
C34 C33 C32 119.6(6) . . ?
C33 C34 N5 122.4(5) . . ?
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
Mo1 N1 2.002(4) . ?
Mo1 N8 2.015(4) . ?
Mo1 N7 2.019(3) . ?
Mo1 N2 2.029(3) . ?
Mo1 N5 2.092(4) . ?
Mo1 N4 2.104(3) . ?
S1 C35 1.735(10) . ?
S1 C6 1.769(7) . ?
S2 C19 1.765(5) . ?
S2 C36 1.781(6) . ?
N1 C7 1.394(6) . ?
N1 C1 1.448(6) . ?
N2 N3 1.345(5) . ?
N2 C12 1.397(6) . ?
N3 C13 1.327(6) . ?
N4 C17 1.366(6) . ?
N4 C13 1.388(6) . ?
N5 C34 1.368(6) . ?
N5 C30 1.383(6) . ?
N6 C30 1.331(6) . ?
N6 N7 1.353(5) . ?
N7 C29 1.405(6) . ?
N8 C24 1.406(5) . ?
N8 C18 1.434(5) . ?
C1 C6 1.340(8) . ?
C1 C2 1.453(7) . ?
C2 C3 1.386(8) . ?
C3 C4 1.414(11) . ?
C4 C5 1.327(11) . ?
C5 C6 1.398(8) . ?
C7 C8 1.400(7) . ?
C7 C12 1.408(6) . ?
C8 C9 1.384(7) . ?
C9 C10 1.368(8) . ?
C10 C11 1.381(8) . ?
C11 C12 1.381(6) . ?
C13 C14 1.409(6) . ?
C14 C15 1.338(9) . ?
C15 C16 1.397(9) . ?
C16 C17 1.351(7) . ?
C18 C19 1.377(6) . ?
C18 C23 1.399(6) . ?
C19 C20 1.397(7) . ?
C20 C21 1.372(9) . ?
C21 C22 1.375(9) . ?
C22 C23 1.345(7) . ?
C24 C25 1.378(6) . ?
C24 C29 1.397(6) . ?
C25 C26 1.388(6) . ?
C26 C27 1.363(7) . ?
C27 C28 1.394(7) . ?
C28 C29 1.382(6) . ?
C30 C31 1.411(7) . ?
C31 C32 1.359(9) . ?
C32 C33 1.404(9) . ?
C33 C34 1.339(8) . ?
