#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/50/7055092.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_7055092
loop_
_publ_author_name
'Biswal, Debanjana'
'Pramanik, Nikhil Ranjan'
'Chakrabarti, Syamal'
'Drew, Michael G. B.'
'Mitra, Payel'
'Acharya, Krishnendu'
'Biswas, Sujan'
'Mondal, Tapan Kumar'
_publ_section_title
;
 Supramolecular frameworks of binuclear dioxomolybdenum(vi) complexes with
 ONS donor ligands using 4,4′-azopyridine as a pillar: crystal
 structure, DFT calculations and biological study
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              8681
_journal_paper_doi               10.1039/C5NJ01899D
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C42 H32 Cl6 Mo2 N10 O10 S4'
_chemical_formula_weight         1369.60
_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
_audit_update_record
;
2015-08-24 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                67.269(6)
_cell_angle_beta                 69.255(5)
_cell_angle_gamma                67.937(6)
_cell_formula_units_Z            1
_cell_length_a                   10.9255(7)
_cell_length_b                   10.9637(7)
_cell_length_c                   13.2353(8)
_cell_measurement_reflns_used    9331
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.33
_cell_volume                     1314.00(16)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9331
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.33
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.214
_refine_diff_density_min         -2.235
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7348
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+2.0871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                5698
_reflns_number_total             7678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01899d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7055090--7055092.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7055092
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 0.43474(4) 0.35831(4) 0.82155(3) 0.01647(12) Uani 1 1 d . . .
O2 O 0.3584(4) 0.3011(4) 0.7625(3) 0.0227(7) Uani 1 1 d . . .
O3 O 0.3064(4) 0.4559(4) 0.9000(3) 0.0267(8) Uani 1 1 d . . .
S1 S 0.48144(13) 0.53705(13) 0.64591(10) 0.0217(3) Uani 1 1 d . . .
N5 N 0.7193(5) 0.0862(5) 1.2986(4) 0.0276(10) Uani 1 1 d . . .
O4 O 0.7139(5) -0.0207(4) 1.3757(3) 0.0420(11) Uani 1 1 d . . .
O5 O 0.7747(5) 0.1675(4) 1.2940(3) 0.0406(11) Uani 1 1 d . . .
C8 C 0.5837(5) 0.6001(5) 0.6783(4) 0.0183(9) Uani 1 1 d . . .
N2 N 0.6310(4) 0.5502(4) 0.7672(3) 0.0186(8) Uani 1 1 d . . .
N1 N 0.5888(4) 0.4339(4) 0.8446(3) 0.0155(8) Uani 1 1 d . . .
C7 C 0.6320(5) 0.3890(5) 0.9351(4) 0.0173(9) Uani 1 1 d . . .
H7 H 0.6821 0.4379 0.9401 0.021 Uiso 1 1 calc R . .
C6 C 0.6095(5) 0.2696(5) 1.0292(4) 0.0163(9) Uani 1 1 d . . .
C5 C 0.6663(5) 0.2368(5) 1.1195(4) 0.0199(10) Uani 1 1 d . . .
H5 H 0.7112 0.2938 1.1198 0.024 Uiso 1 1 calc R . .
C4 C 0.6547(5) 0.1191(5) 1.2076(4) 0.0193(10) Uani 1 1 d . . .
C3 C 0.5912(6) 0.0300(5) 1.2113(4) 0.0236(11) Uani 1 1 d . . .
H3 H 0.5866 -0.0494 1.2716 0.028 Uiso 1 1 calc R . .
C2 C 0.5343(6) 0.0613(5) 1.1231(4) 0.0232(10) Uani 1 1 d . . .
H2 H 0.4897 0.0027 1.1250 0.028 Uiso 1 1 calc R . .
C1 C 0.5426(5) 0.1795(5) 1.0310(4) 0.0172(9) Uani 1 1 d . . .
O1 O 0.4943(4) 0.1999(3) 0.9458(3) 0.0189(7) Uani 1 1 d . . .
N3 N 0.6415(4) 0.2219(4) 0.7249(3) 0.0170(8) Uani 1 1 d . . .
C16 C 0.7528(5) 0.1515(5) 0.7658(4) 0.0219(10) Uani 1 1 d . . .
H16 H 0.7504 0.1544 0.8358 0.026 Uiso 1 1 calc R . .
C17 C 0.8697(5) 0.0756(6) 0.7097(4) 0.0259(11) Uani 1 1 d . . .
H17 H 0.9444 0.0276 0.7412 0.031 Uiso 1 1 calc R . .
C18 C 0.8735(5) 0.0727(5) 0.6045(4) 0.0208(10) Uani 1 1 d . . .
C19 C 0.7593(5) 0.1423(5) 0.5615(4) 0.0194(10) Uani 1 1 d . . .
H19 H 0.7590 0.1402 0.4920 0.023 Uiso 1 1 calc R . .
C20 C 0.6466(5) 0.2142(5) 0.6241(4) 0.0196(9) Uani 1 1 d . . .
H20 H 0.5695 0.2603 0.5956 0.024 Uiso 1 1 calc R . .
N4 N 1.0014(5) -0.0002(5) 0.5455(4) 0.0280(10) Uani 1 1 d . . .
S2 S 0.62006(13) 0.74686(13) 0.57280(10) 0.0216(3) Uani 1 1 d . . .
C9 C 0.7223(6) 0.7920(5) 0.6291(4) 0.0245(11) Uani 1 1 d . . .
H9B H 0.7192 0.8881 0.5914 0.029 Uiso 1 1 calc R . .
H9A H 0.6795 0.7829 0.7086 0.029 Uiso 1 1 calc R . .
C10 C 0.8688(6) 0.7098(5) 0.6181(4) 0.0263(11) Uani 1 1 d . . .
C15 C 0.9484(6) 0.6739(6) 0.5197(5) 0.0325(13) Uani 1 1 d . . .
H15 H 0.9092 0.6983 0.4602 0.039 Uiso 1 1 calc R . .
C14 C 1.0855(7) 0.6022(7) 0.5092(6) 0.0398(15) Uani 1 1 d . . .
H14 H 1.1366 0.5769 0.4437 0.048 Uiso 1 1 calc R . .
C13 C 1.1460(7) 0.5684(7) 0.5956(6) 0.0449(16) Uani 1 1 d . . .
H13 H 1.2378 0.5208 0.5885 0.054 Uiso 1 1 calc R . .
C12 C 1.0694(7) 0.6058(7) 0.6927(6) 0.0469(18) Uani 1 1 d . . .
H12 H 1.1102 0.5852 0.7504 0.056 Uiso 1 1 calc R . .
C11 C 0.9306(7) 0.6747(6) 0.7043(5) 0.0375(14) Uani 1 1 d . . .
H11 H 0.8792 0.6973 0.7708 0.045 Uiso 1 1 calc R . .
C1A C 0.9254(14) 0.7185(15) 0.1032(11) 0.046(3) Uiso 0.526(6) 1 d PD A 1
H1A H 0.8583 0.6680 0.1535 0.055 Uiso 0.526(6) 1 calc PR A 1
Cl1A Cl 0.8438(4) 0.8628(4) 0.0040(3) 0.0714(18) Uani 0.526(6) 1 d PD A 1
Cl2A Cl 1.0041(3) 0.7430(3) 0.1906(2) 0.0954(10) Uani 0.526(6) 1 d PD A 1
Cl3A Cl 1.0363(3) 0.6261(3) 0.02310(17) 0.0809(8) Uani 0.526(6) 1 d PD A 1
Cl1B Cl 0.9327(6) 0.9376(5) 0.0131(5) 0.089(2) Uani 0.474(6) 1 d PD . 2
Cl2B Cl 1.0041(3) 0.7430(3) 0.1906(2) 0.0954(10) Uani 0.474(6) 1 d PD A 2
Cl3B Cl 1.0363(3) 0.6261(3) 0.02310(17) 0.0809(8) Uani 0.474(6) 1 d PD A 2
C1B C 0.9284(17) 0.7668(15) 0.0947(12) 0.049(4) Uiso 0.474(6) 1 d PD A 2
H1B H 0.8346 0.7606 0.1289 0.058 Uiso 0.474(6) 1 calc PR A 2
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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O3 Mo1 O2 106.18(17) .
O3 Mo1 O1 98.31(16) .
O2 Mo1 O1 105.31(15) .
O3 Mo1 N1 89.86(16) .
O2 Mo1 N1 160.95(15) .
O1 Mo1 N1 81.87(14) .
O3 Mo1 N3 170.63(16) .
O2 Mo1 N3 83.03(15) .
O1 Mo1 N3 77.17(13) .
N1 Mo1 N3 81.42(13) .
O3 Mo1 S1 99.66(14) .
O2 Mo1 S1 90.76(12) .
O1 Mo1 S1 151.43(11) .
N1 Mo1 S1 76.16(10) .
N3 Mo1 S1 81.65(10) .
C8 S1 Mo1 100.10(16) .
O5 N5 O4 123.5(5) .
O5 N5 C4 118.3(4) .
O4 N5 C4 118.2(4) .
N2 C8 S2 120.6(4) .
N2 C8 S1 127.5(4) .
S2 C8 S1 111.9(3) .
C8 N2 N1 113.0(4) .
C7 N1 N2 112.2(4) .
C7 N1 Mo1 124.6(3) .
N2 N1 Mo1 122.5(3) .
N1 C7 C6 125.9(4) .
C5 C6 C1 118.9(4) .
C5 C6 C7 117.2(4) .
C1 C6 C7 123.7(4) .
C4 C5 C6 119.1(4) .
C3 C4 C5 123.2(4) .
C3 C4 N5 119.4(4) .
C5 C4 N5 117.4(4) .
C4 C3 C2 118.4(5) .
C3 C2 C1 121.2(5) .
O1 C1 C2 118.8(4) .
O1 C1 C6 121.9(4) .
C2 C1 C6 119.2(4) .
C1 O1 Mo1 135.9(3) .
C16 N3 C20 117.1(4) .
C16 N3 Mo1 124.1(3) .
C20 N3 Mo1 118.8(3) .
N3 C16 C17 123.5(4) .
C16 C17 C18 118.1(5) .
C19 C18 C17 119.5(4) .
C19 C18 N4 124.4(4) .
C17 C18 N4 116.1(4) .
C20 C19 C18 118.2(4) .
N3 C20 C19 123.5(5) .
N4 N4 C18 113.2(6) 2_756
C8 S2 C9 102.6(2) .
C10 C9 S2 116.8(4) .
C11 C10 C15 118.2(6) .
C11 C10 C9 120.1(5) .
C15 C10 C9 121.6(5) .
C14 C15 C10 121.0(6) .
C13 C14 C15 120.2(6) .
C12 C13 C14 119.6(6) .
C13 C12 C11 120.1(6) .
C10 C11 C12 120.9(6) .
Cl3A C1A Cl1A 101.9(7) .
Cl3A C1A Cl2A 111.0(8) .
Cl1A C1A Cl2A 120.4(8) .
Cl2B C1B Cl1B 100.1(8) .
Cl2B C1B Cl3B 105.4(8) .
Cl1B C1B Cl3B 116.7(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.700(3) .
Mo1 O2 1.713(3) .
Mo1 O1 1.961(3) .
Mo1 N1 2.285(4) .
Mo1 N3 2.423(4) .
Mo1 S1 2.4280(13) .
S1 C8 1.748(5) .
N5 O5 1.226(6) .
N5 O4 1.226(6) .
N5 C4 1.468(6) .
C8 N2 1.293(6) .
C8 S2 1.746(5) .
N2 N1 1.409(5) .
N1 C7 1.292(6) .
C7 C6 1.445(6) .
C6 C5 1.403(6) .
C6 C1 1.423(7) .
C5 C4 1.377(7) .
C4 C3 1.373(7) .
C3 C2 1.382(7) .
C2 C1 1.401(7) .
C1 O1 1.318(5) .
N3 C16 1.343(6) .
N3 C20 1.350(6) .
C16 C17 1.372(7) .
C17 C18 1.391(7) .
C18 C19 1.385(7) .
C18 N4 1.439(6) .
C19 C20 1.370(6) .
N4 N4 1.214(8) 2_756
S2 C9 1.826(5) .
C9 C10 1.499(8) .
C10 C11 1.384(8) .
C10 C15 1.395(8) .
C15 C14 1.390(9) .
C14 C13 1.381(9) .
C13 C12 1.381(10) .
C12 C11 1.399(9) .
C1A Cl3A 1.618(13) .
C1A Cl1A 1.785(13) .
C1A Cl2A 1.808(13) .
Cl1B C1B 1.773(15) .
Cl2B C1B 1.639(14) .
Cl3B C1B 1.908(14) .
