 
data_mo_CHEM0048_b0ma
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          '2(C37 H35 N5 S2), 3(C7 H8)'
_chemical_formula_sum
 'C95 H94 N10 S4' 
_chemical_formula_weight          1504.04

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'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    7.976(3)
_cell_length_b                    11.054(4)
_cell_length_c                    22.319(7)
_cell_angle_alpha                 79.904(9)
_cell_angle_beta                  80.498(10)
_cell_angle_gamma                 82.348(9)
_cell_volume                      1899.8(11)
_cell_formula_units_Z             1
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9964
_cell_measurement_theta_min       2.44
_cell_measurement_theta_max       29.98
 
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.315          
_exptl_crystal_F_000              798
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.319
_exptl_crystal_size_mid           0.222
_exptl_crystal_size_min           0.086
_exptl_absorpt_coefficient_mu     0.183
_shelx_estimated_absorpt_T_min    0.944
_shelx_estimated_absorpt_T_max    0.984
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6445  
_exptl_absorpt_correction_T_max   0.7460
_exptl_absorpt_process_details    'SADABS (Sheldrick, 2015)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'microfocus I\mS'
_diffrn_measurement_device_type   
'Bruker D8 Venture with Photon100 CMOS detector'
_diffrn_measurement_method        'ω and φ scans'
_diffrn_detector_area_resol_mean  1024
_diffrn_reflns_number             43507
_diffrn_reflns_av_unetI/netI      0.0971
_diffrn_reflns_av_R_equivalents   0.2361
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          2.604
_diffrn_reflns_theta_max          25.027
_diffrn_reflns_theta_full         25.027
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              6708
_reflns_number_gt                 5535
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_cell_refinement        'SAINT v8.34A (Bruker, 2014)'
_computing_data_reduction         'SAINT v8.34A (Bruker, 2014)'
_computing_structure_solution     'XT (Sheldrick, 2015)'
_computing_structure_refinement   'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'Mercury (Macrae et. al, 2008)'
_computing_publication_material   'XL (Sheldrick, 2008)'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+2.2505P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          6708
_refine_ls_number_parameters      540
_refine_ls_number_restraints      49
_refine_ls_R_factor_all           0.0785
_refine_ls_R_factor_gt            0.0632
_refine_ls_wR_factor_ref          0.1678
_refine_ls_wR_factor_gt           0.1567
_refine_ls_goodness_of_fit_ref    1.113
_refine_ls_restrained_S_all       1.110
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1 S 0.08406(9) 0.37420(6) 0.38301(3) 0.0207(2) Uani 1 1 d . . . . .
S2 S 0.05080(9) 0.14107(6) 0.51177(3) 0.0217(2) Uani 1 1 d . . . . .
N1 N 0.3236(3) 0.6081(2) 0.51273(11) 0.0195(5) Uani 1 1 d . . . . .
N2 N 0.4298(3) 0.7287(2) 0.56859(11) 0.0202(5) Uani 1 1 d . . . . .
N3 N 0.4072(3) 0.5391(2) 0.67218(11) 0.0212(5) Uani 1 1 d . . . . .
N4 N 0.3059(3) 0.4152(2) 0.61628(11) 0.0205(5) Uani 1 1 d . . . . .
N5 N 0.604(4) 0.9945(12) 0.6887(6) 0.0250(11) Uani 0.62(3) 1 d . . P A 1
C32 C 0.582(2) 0.8104(9) 0.7921(5) 0.018(4) Uani 0.62(3) 1 d D . P A 1
H32 H 0.6140 0.8887 0.7950 0.022 Uiso 0.62(3) 1 calc R U P A 1
C32B C 0.599(9) 0.995(2) 0.6927(12) 0.0250(11) Uani 0.38(3) 1 d D . P A 2
H32B H 0.6130 1.0118 0.7319 0.030 Uiso 0.38(3) 1 calc R U P A 2
N5B N 0.571(3) 0.8078(19) 0.7947(9) 0.042(8) Uani 0.38(3) 1 d . . P A 2
C1 C 0.3295(4) 1.0282(3) 0.08152(15) 0.0347(8) Uani 1 1 d . . . . .
H1A H 0.3411 1.0437 0.0365 0.052 Uiso 1 1 calc R U . . .
H1B H 0.4384 1.0368 0.0944 0.052 Uiso 1 1 calc R U . . .
H1C H 0.2402 1.0881 0.0984 0.052 Uiso 1 1 calc R U . . .
C2 C 0.2815(4) 0.8986(3) 0.10505(14) 0.0308(7) Uani 1 1 d . . . . .
H2A H 0.1722 0.8906 0.0913 0.037 Uiso 1 1 calc R U . . .
H2B H 0.3702 0.8391 0.0865 0.037 Uiso 1 1 calc R U . . .
C3 C 0.2625(4) 0.8645(3) 0.17431(14) 0.0260(7) Uani 1 1 d . . . . .
H3A H 0.3741 0.8669 0.1878 0.031 Uiso 1 1 calc R U . . .
H3B H 0.1798 0.9274 0.1929 0.031 Uiso 1 1 calc R U . . .
C4 C 0.2031(4) 0.7385(3) 0.19831(14) 0.0263(7) Uani 1 1 d . . . . .
H4A H 0.2779 0.6769 0.1760 0.032 Uiso 1 1 calc R U . . .
H4B H 0.0856 0.7393 0.1891 0.032 Uiso 1 1 calc R U . . .
C5 C 0.2033(4) 0.6978(3) 0.26702(14) 0.0252(7) Uani 1 1 d . . . . .
H5A H 0.1419 0.7645 0.2893 0.030 Uiso 1 1 calc R U . . .
H5B H 0.3228 0.6847 0.2757 0.030 Uiso 1 1 calc R U . . .
C6 C 0.1192(4) 0.5795(3) 0.29094(13) 0.0243(6) Uani 1 1 d . . . . .
H6A H -0.0047 0.5974 0.2886 0.029 Uiso 1 1 calc R U . . .
H6B H 0.1666 0.5181 0.2635 0.029 Uiso 1 1 calc R U . . .
C7 C 0.1420(3) 0.5231(3) 0.35543(13) 0.0202(6) Uani 1 1 d . . . . .
C8 C 0.2051(3) 0.5685(3) 0.39919(13) 0.0202(6) Uani 1 1 d . . . . .
H8 H 0.2443 0.6479 0.3927 0.024 Uiso 1 1 calc R U . . .
C9 C 0.2062(3) 0.4846(3) 0.45579(13) 0.0202(6) Uani 1 1 d . . . . .
C10 C 0.1430(3) 0.3751(3) 0.45382(13) 0.0197(6) Uani 1 1 d . . . . .
C11 C 0.1325(3) 0.2799(2) 0.50526(13) 0.0197(6) Uani 1 1 d . . . . .
C12 C 0.1896(3) 0.2916(3) 0.55923(13) 0.0210(6) Uani 1 1 d . . . . .
C13 C 0.1668(3) 0.1853(3) 0.60529(14) 0.0217(6) Uani 1 1 d . . . . .
H13 H 0.1982 0.1780 0.6451 0.026 Uiso 1 1 calc R U . . .
C14 C 0.0960(3) 0.0958(3) 0.58669(13) 0.0209(6) Uani 1 1 d . . . . .
C15 C 0.0619(4) -0.0309(3) 0.61923(14) 0.0229(6) Uani 1 1 d . . . . .
H15A H 0.1423 -0.0924 0.5987 0.027 Uiso 1 1 calc R U . . .
H15B H -0.0553 -0.0446 0.6149 0.027 Uiso 1 1 calc R U . . .
C16 C 0.0790(4) -0.0540(3) 0.68718(14) 0.0243(7) Uani 1 1 d . . . . .
H16A H -0.0025 0.0060 0.7084 0.029 Uiso 1 1 calc R U . . .
H16B H 0.1960 -0.0408 0.6921 0.029 Uiso 1 1 calc R U . . .
C17 C 0.0439(4) -0.1846(3) 0.71685(14) 0.0248(7) Uani 1 1 d . . . . .
H17A H -0.0734 -0.1967 0.7116 0.030 Uiso 1 1 calc R U . . .
H17B H 0.1242 -0.2438 0.6947 0.030 Uiso 1 1 calc R U . . .
C18 C 0.0603(4) -0.2153(3) 0.78450(14) 0.0279(7) Uani 1 1 d . . . . .
H18A H -0.0221 -0.1579 0.8070 0.034 Uiso 1 1 calc R U . . .
H18B H 0.1767 -0.2020 0.7900 0.034 Uiso 1 1 calc R U . . .
C19 C 0.0281(4) -0.3472(3) 0.81233(16) 0.0326(8) Uani 1 1 d . . . . .
H19A H -0.0859 -0.3620 0.8049 0.039 Uiso 1 1 calc R U . . .
H19B H 0.1145 -0.4048 0.7914 0.039 Uiso 1 1 calc R U . . .
C20 C 0.0355(5) -0.3749(3) 0.88048(17) 0.0454(9) Uani 1 1 d . . . . .
H20A H 0.1518 -0.3695 0.8879 0.068 Uiso 1 1 calc R U . . .
H20B H 0.0040 -0.4584 0.8966 0.068 Uiso 1 1 calc R U . . .
H20C H -0.0444 -0.3148 0.9013 0.068 Uiso 1 1 calc R U . . .
C21 C 0.2643(3) 0.5026(2) 0.51110(13) 0.0187(6) Uani 1 1 d . . . . .
C22 C 0.2557(3) 0.4035(3) 0.56392(13) 0.0204(6) Uani 1 1 d . . . . .
C23 C 0.3725(3) 0.6200(3) 0.56631(13) 0.0189(6) Uani 1 1 d . . . . .
C24 C 0.3630(3) 0.5239(2) 0.61806(13) 0.0194(6) Uani 1 1 d . . . . .
C25 C 0.4746(3) 0.7418(3) 0.62156(13) 0.0192(6) Uani 1 1 d . . . . .
C26 C 0.5318(3) 0.8591(3) 0.62659(13) 0.0199(6) Uani 1 1 d . . . . .
C27 C 0.5514(3) 0.9521(3) 0.57588(14) 0.0233(6) Uani 1 1 d . . . . .
H27 H 0.5357 0.9371 0.5367 0.028 Uiso 1 1 calc R U . . .
C28 C 0.5935(4) 1.0656(3) 0.58218(14) 0.0249(7) Uani 1 1 d D . . . .
H28 H 0.6066 1.1297 0.5479 0.030 Uiso 1 1 calc R U . . .
C29 C 0.6161(4) 1.0833(3) 0.64022(14) 0.0276(7) Uani 1 1 d D . . . .
H29 H 0.6411 1.1621 0.6455 0.033 Uiso 1 1 calc R U . A 1
C30 C 0.5614(3) 0.8818(3) 0.68359(14) 0.0225(6) Uani 1 1 d D . . . .
C31 C 0.5477(3) 0.7849(3) 0.73725(13) 0.0220(6) Uani 1 1 d D . . . .
C33 C 0.5670(4) 0.7184(3) 0.84276(15) 0.0281(7) Uani 1 1 d D . . . .
H33 H 0.5840 0.7360 0.8814 0.034 Uiso 1 1 calc R U . A 1
C34 C 0.5283(4) 0.6014(3) 0.83932(15) 0.0288(7) Uani 1 1 d . . . . .
H34 H 0.5233 0.5393 0.8747 0.035 Uiso 1 1 calc R U . . .
C35 C 0.4972(4) 0.5762(3) 0.78428(14) 0.0261(7) Uani 1 1 d . . . . .
H35 H 0.4709 0.4963 0.7815 0.031 Uiso 1 1 calc R U . . .
C36 C 0.5043(3) 0.6686(3) 0.73209(13) 0.0213(6) Uani 1 1 d . . . . .
C37 C 0.4624(3) 0.6458(2) 0.67390(13) 0.0192(6) Uani 1 1 d . . . . .
C38 C 0.1803(5) -0.0426(4) 0.9232(2) 0.0569(11) Uani 1 1 d D . . . .
H38A H 0.2684 -0.1094 0.9129 0.085 Uiso 1 1 calc R U . . .
H38B H 0.0679 -0.0647 0.9196 0.085 Uiso 1 1 calc R U . . .
H38C H 0.1816 -0.0299 0.9655 0.085 Uiso 1 1 calc R U . . .
C39 C 0.2157(4) 0.0749(3) 0.87965(17) 0.0364(8) Uani 1 1 d D . . . .
C40 C 0.2528(4) 0.0744(3) 0.81740(17) 0.0389(9) Uani 1 1 d D . . . .
H40 H 0.2573 -0.0011 0.8021 0.047 Uiso 1 1 calc R U . . .
C41 C 0.2835(4) 0.1805(3) 0.77669(17) 0.0397(8) Uani 1 1 d D . . . .
H41 H 0.3091 0.1775 0.7338 0.048 Uiso 1 1 calc R U . . .
C42 C 0.2774(4) 0.2907(3) 0.79760(18) 0.0409(9) Uani 1 1 d D . . . .
H42 H 0.2967 0.3643 0.7695 0.049 Uiso 1 1 calc R U . . .
C43 C 0.2429(5) 0.2932(3) 0.86008(18) 0.0438(9) Uani 1 1 d D . . . .
H43 H 0.2401 0.3688 0.8751 0.053 Uiso 1 1 calc R U . . .
C44 C 0.2124(4) 0.1866(3) 0.90076(17) 0.0412(9) Uani 1 1 d D . . . .
H44 H 0.1888 0.1894 0.9437 0.049 Uiso 1 1 calc R U . . .
C45 C 0.1874(9) 0.6443(6) 1.0237(3) 0.0414(17) Uani 0.5 1 d D . P B -1
H45A H 0.0986 0.6228 1.0031 0.062 Uiso 0.5 1 calc R U P B -1
H45B H 0.2087 0.7304 1.0084 0.062 Uiso 0.5 1 calc R U P B -1
H45C H 0.1494 0.6342 1.0681 0.062 Uiso 0.5 1 calc R U P B -1
C46 C 0.3501(16) 0.5604(13) 1.0104(11) 0.030(3) Uani 0.5 1 d D U P B -1
C47 C 0.5086(18) 0.5994(12) 1.0094(10) 0.038(3) Uani 0.5 1 d D U P B -1
H47 H 0.5160 0.6813 1.0156 0.046 Uiso 0.5 1 calc R U P B -1
C48 C 0.656(2) 0.5204(14) 0.9994(11) 0.043(4) Uani 0.5 1 d D U P B -1
H48 H 0.7638 0.5488 0.9985 0.052 Uiso 0.5 1 calc R U P B -1
C49 C 0.649(2) 0.4001(15) 0.9906(13) 0.053(5) Uani 0.5 1 d D . P B -1
H49 H 0.7504 0.3456 0.9840 0.064 Uiso 0.5 1 calc R U P B -1
C50 C 0.491(2) 0.3617(12) 0.9918(11) 0.044(4) Uani 0.5 1 d D U P B -1
H50 H 0.4841 0.2794 0.9860 0.053 Uiso 0.5 1 calc R U P B -1
C51 C 0.344(2) 0.4390(12) 1.0009(10) 0.031(3) Uani 0.5 1 d D . P B -1
H51 H 0.2372 0.4104 1.0008 0.037 Uiso 0.5 1 calc R U P B -1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
S1 C10 1.723(3) . ?
S1 C7 1.748(3) . ?
S2 C11 1.720(3) . ?
S2 C14 1.742(3) . ?
N1 C21 1.323(4) . ?
N1 C23 1.350(4) . ?
N2 C25 1.326(4) . ?
N2 C23 1.353(4) . ?
N3 C37 1.322(4) . ?
N3 C24 1.356(4) . ?
N4 C22 1.329(4) . ?
N4 C24 1.350(4) . ?
N5 C29 1.327(11) . ?
N5 C30 1.364(10) . ?
C32 C31 1.380(11) . ?
C32 C33 1.382(11) . ?
C32 H32 0.9500 . ?
C32B C29 1.384(17) . ?
C32B C30 1.387(17) . ?
C32B H32B 0.9500 . ?
N5B C33 1.32(2) . ?
N5B C31 1.397(19) . ?
C1 C2 1.514(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.513(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.510(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.521(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.523(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.495(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.363(4) . ?
C8 C9 1.431(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(4) . ?
C9 C21 1.442(4) . ?
C10 C11 1.414(4) . ?
C11 C12 1.388(4) . ?
C12 C13 1.429(4) . ?
C12 C22 1.433(4) . ?
C13 C14 1.356(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.497(4) . ?
C15 C16 1.519(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.521(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.512(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.518(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.508(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.462(4) . ?
C23 C24 1.425(4) . ?
C25 C37 1.434(4) . ?
C25 C26 1.459(4) . ?
C26 C27 1.392(4) . ?
C26 C30 1.402(4) . ?
C27 C28 1.377(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.460(4) . ?
C31 C36 1.404(4) . ?
C33 C34 1.387(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.374(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.407(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.464(4) . ?
C38 C39 1.509(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.373(5) . ?
C39 C44 1.392(5) . ?
C40 C41 1.376(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.371(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.381(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.379(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.510(12) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.385(14) . ?
C46 C51 1.403(13) . ?
C47 C48 1.379(14) . ?
C47 H47 0.9500 . ?
C48 C49 1.388(14) . ?
C48 H48 0.9500 . ?
C49 C50 1.377(15) . ?
C49 H49 0.9500 . ?
C50 C51 1.362(14) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
 
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
C10 S1 C7 92.05(13) . . ?
C11 S2 C14 92.15(14) . . ?
C21 N1 C23 116.3(2) . . ?
C25 N2 C23 116.7(2) . . ?
C37 N3 C24 116.7(2) . . ?
C22 N4 C24 116.3(2) . . ?
C29 N5 C30 120.4(10) . . ?
C31 C32 C33 117.7(9) . . ?
C31 C32 H32 121.1 . . ?
C33 C32 H32 121.1 . . ?
C29 C32B C30 114.9(17) . . ?
C29 C32B H32B 122.6 . . ?
C30 C32B H32B 122.6 . . ?
C33 N5B C31 120.7(15) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 113.8(3) . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 114.0(2) . . ?
C4 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 114.1(2) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C4 C5 C6 112.4(2) . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
C7 C6 C5 114.8(2) . . ?
C7 C6 H6A 108.6 . . ?
C5 C6 H6A 108.6 . . ?
C7 C6 H6B 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
C8 C7 C6 130.5(3) . . ?
C8 C7 S1 110.9(2) . . ?
C6 C7 S1 118.6(2) . . ?
C7 C8 C9 113.2(3) . . ?
C7 C8 H8 123.4 . . ?
C9 C8 H8 123.4 . . ?
C10 C9 C8 112.5(2) . . ?
C10 C9 C21 119.7(3) . . ?
C8 C9 C21 127.8(3) . . ?
C9 C10 C11 121.4(3) . . ?
C9 C10 S1 111.3(2) . . ?
C11 C10 S1 127.3(2) . . ?
C12 C11 C10 121.2(3) . . ?
C12 C11 S2 111.2(2) . . ?
C10 C11 S2 127.6(2) . . ?
C11 C12 C13 112.1(2) . . ?
C11 C12 C22 119.7(3) . . ?
C13 C12 C22 128.2(3) . . ?
C14 C13 C12 113.6(3) . . ?
C14 C13 H13 123.2 . . ?
C12 C13 H13 123.2 . . ?
C13 C14 C15 130.0(3) . . ?
C13 C14 S2 111.0(2) . . ?
C15 C14 S2 119.0(2) . . ?
C14 C15 C16 114.7(2) . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15B 108.6 . . ?
C16 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 C17 111.6(2) . . ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 114.8(2) . . ?
C18 C17 H17A 108.6 . . ?
C16 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
C16 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 C19 113.4(3) . . ?
C17 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 113.0(3) . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C18 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 C9 119.3(3) . . ?
N1 C21 C22 121.9(3) . . ?
C9 C21 C22 118.8(2) . . ?
N4 C22 C12 119.3(3) . . ?
N4 C22 C21 121.5(3) . . ?
C12 C22 C21 119.1(2) . . ?
N1 C23 N2 116.5(3) . . ?
N1 C23 C24 121.9(2) . . ?
N2 C23 C24 121.5(3) . . ?
N4 C24 N3 116.8(3) . . ?
N4 C24 C23 122.0(3) . . ?
N3 C24 C23 121.2(2) . . ?
N2 C25 C37 121.7(3) . . ?
N2 C25 C26 118.4(3) . . ?
C37 C25 C26 119.8(2) . . ?
C27 C26 C30 118.8(3) . . ?
C27 C26 C25 121.1(3) . . ?
C30 C26 C25 120.1(3) . . ?
C28 C27 C26 120.5(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 117.8(3) . . ?
C27 C28 H28 121.1 . . ?
C29 C28 H28 121.1 . . ?
N5 C29 C28 122.7(6) . . ?
C32B C29 C28 125.0(9) . . ?
N5 C29 H29 118.7 . . ?
C28 C29 H29 118.7 . . ?
N5 C30 C26 119.8(6) . . ?
C32B C30 C26 122.9(10) . . ?
N5 C30 C31 120.0(6) . . ?
C32B C30 C31 116.9(9) . . ?
C26 C30 C31 120.2(3) . . ?
C32 C31 C36 121.6(5) . . ?
N5B C31 C36 119.1(9) . . ?
C32 C31 C30 118.2(5) . . ?
N5B C31 C30 120.7(9) . . ?
C36 C31 C30 120.2(3) . . ?
N5B C33 C34 121.8(9) . . ?
C32 C33 C34 122.5(5) . . ?
C32 C33 H33 118.8 . . ?
C34 C33 H33 118.8 . . ?
C35 C34 C33 119.3(3) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C31 C36 C35 118.6(3) . . ?
C31 C36 C37 120.3(3) . . ?
C35 C36 C37 121.0(3) . . ?
N3 C37 C25 122.2(3) . . ?
N3 C37 C36 118.7(3) . . ?
C25 C37 C36 119.1(2) . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 117.9(3) . . ?
C40 C39 C38 120.4(3) . . ?
C44 C39 C38 121.7(4) . . ?
C39 C40 C41 121.5(3) . . ?
C39 C40 H40 119.2 . . ?
C41 C40 H40 119.2 . . ?
C42 C41 C40 120.4(3) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 119.1(3) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C44 C43 C42 120.3(3) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C39 120.7(3) . . ?
C43 C44 H44 119.6 . . ?
C39 C44 H44 119.6 . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 C51 118.1(11) . . ?
C47 C46 C45 121.1(12) . . ?
C51 C46 C45 120.7(10) . . ?
C48 C47 C46 120.6(12) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C47 C48 C49 120.9(13) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 H48 119.6 . . ?
C50 C49 C48 118.3(14) . . ?
C50 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
C51 C50 C49 121.5(13) . . ?
C51 C50 H50 119.3 . . ?
C49 C50 H50 119.3 . . ?
C50 C51 C46 120.6(12) . . ?
C50 C51 H51 119.7 . . ?
C46 C51 H51 119.7 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C1 C2 C3 C4 176.1(3) . . . . ?
C2 C3 C4 C5 173.4(2) . . . . ?
C3 C4 C5 C6 171.9(2) . . . . ?
C4 C5 C6 C7 170.0(2) . . . . ?
C5 C6 C7 C8 10.2(4) . . . . ?
C5 C6 C7 S1 -169.0(2) . . . . ?
C10 S1 C7 C8 0.7(2) . . . . ?
C10 S1 C7 C6 -180.0(2) . . . . ?
C6 C7 C8 C9 -179.8(3) . . . . ?
S1 C7 C8 C9 -0.6(3) . . . . ?
C7 C8 C9 C10 0.1(3) . . . . ?
C7 C8 C9 C21 179.8(3) . . . . ?
C8 C9 C10 C11 -179.7(2) . . . . ?
C21 C9 C10 C11 0.5(4) . . . . ?
C8 C9 C10 S1 0.4(3) . . . . ?
C21 C9 C10 S1 -179.3(2) . . . . ?
C7 S1 C10 C9 -0.6(2) . . . . ?
C7 S1 C10 C11 179.5(3) . . . . ?
C9 C10 C11 C12 -1.7(4) . . . . ?
S1 C10 C11 C12 178.1(2) . . . . ?
C9 C10 C11 S2 177.4(2) . . . . ?
S1 C10 C11 S2 -2.7(4) . . . . ?
C14 S2 C11 C12 -1.0(2) . . . . ?
C14 S2 C11 C10 179.7(3) . . . . ?
C10 C11 C12 C13 179.9(2) . . . . ?
S2 C11 C12 C13 0.6(3) . . . . ?
C10 C11 C12 C22 1.9(4) . . . . ?
S2 C11 C12 C22 -177.4(2) . . . . ?
C11 C12 C13 C14 0.4(3) . . . . ?
C22 C12 C13 C14 178.1(3) . . . . ?
C12 C13 C14 C15 175.7(3) . . . . ?
C12 C13 C14 S2 -1.2(3) . . . . ?
C11 S2 C14 C13 1.3(2) . . . . ?
C11 S2 C14 C15 -176.0(2) . . . . ?
C13 C14 C15 C16 12.5(4) . . . . ?
S2 C14 C15 C16 -170.83(19) . . . . ?
C14 C15 C16 C17 -179.6(2) . . . . ?
C15 C16 C17 C18 179.4(2) . . . . ?
C16 C17 C18 C19 -178.8(2) . . . . ?
C17 C18 C19 C20 -177.0(3) . . . . ?
C23 N1 C21 C9 178.6(2) . . . . ?
C23 N1 C21 C22 -1.3(4) . . . . ?
C10 C9 C21 N1 -179.6(2) . . . . ?
C8 C9 C21 N1 0.7(4) . . . . ?
C10 C9 C21 C22 0.4(4) . . . . ?
C8 C9 C21 C22 -179.3(3) . . . . ?
C24 N4 C22 C12 -178.5(2) . . . . ?
C24 N4 C22 C21 0.8(4) . . . . ?
C11 C12 C22 N4 178.3(2) . . . . ?
C13 C12 C22 N4 0.7(4) . . . . ?
C11 C12 C22 C21 -1.0(4) . . . . ?
C13 C12 C22 C21 -178.6(2) . . . . ?
N1 C21 C22 N4 0.5(4) . . . . ?
C9 C21 C22 N4 -179.4(2) . . . . ?
N1 C21 C22 C12 179.8(2) . . . . ?
C9 C21 C22 C12 -0.1(4) . . . . ?
C21 N1 C23 N2 -178.6(2) . . . . ?
C21 N1 C23 C24 0.8(4) . . . . ?
C25 N2 C23 N1 178.6(2) . . . . ?
C25 N2 C23 C24 -0.7(4) . . . . ?
C22 N4 C24 N3 177.1(2) . . . . ?
C22 N4 C24 C23 -1.3(4) . . . . ?
C37 N3 C24 N4 -179.7(2) . . . . ?
C37 N3 C24 C23 -1.3(4) . . . . ?
N1 C23 C24 N4 0.6(4) . . . . ?
N2 C23 C24 N4 179.9(2) . . . . ?
N1 C23 C24 N3 -177.7(2) . . . . ?
N2 C23 C24 N3 1.6(4) . . . . ?
C23 N2 C25 C37 -0.3(4) . . . . ?
C23 N2 C25 C26 -178.0(2) . . . . ?
N2 C25 C26 C27 -4.8(4) . . . . ?
C37 C25 C26 C27 177.4(2) . . . . ?
N2 C25 C26 C30 172.7(2) . . . . ?
C37 C25 C26 C30 -5.2(4) . . . . ?
C30 C26 C27 C28 -2.2(4) . . . . ?
C25 C26 C27 C28 175.3(2) . . . . ?
C26 C27 C28 C29 0.3(4) . . . . ?
C30 N5 C29 C28 -3(4) . . . . ?
C30 C32B C29 C28 2(6) . . . . ?
C27 C28 C29 N5 2.2(19) . . . . ?
C27 C28 C29 C32B 0(4) . . . . ?
C29 N5 C30 C26 1(3) . . . . ?
C29 N5 C30 C31 -179.7(18) . . . . ?
C29 C32B C30 C26 -4(6) . . . . ?
C29 C32B C30 C31 178(3) . . . . ?
C27 C26 C30 N5 1.7(18) . . . . ?
C25 C26 C30 N5 -175.8(17) . . . . ?
C27 C26 C30 C32B 4(3) . . . . ?
C25 C26 C30 C32B -173(3) . . . . ?
C27 C26 C30 C31 -177.9(2) . . . . ?
C25 C26 C30 C31 4.6(4) . . . . ?
C33 C32 C31 C36 -1.7(14) . . . . ?
C33 C32 C31 C30 179.5(7) . . . . ?
C33 N5B C31 C36 6(3) . . . . ?
C33 N5B C31 C30 -176.6(13) . . . . ?
N5 C30 C31 C32 -1.0(19) . . . . ?
C26 C30 C31 C32 178.6(7) . . . . ?
C32B C30 C31 N5B 1(3) . . . . ?
C26 C30 C31 N5B -177.7(12) . . . . ?
N5 C30 C31 C36 -179.8(17) . . . . ?
C32B C30 C31 C36 178(3) . . . . ?
C26 C30 C31 C36 -0.2(4) . . . . ?
C31 N5B C33 C34 -5(3) . . . . ?
C31 C32 C33 C34 3.3(14) . . . . ?
N5B C33 C34 C35 1.6(14) . . . . ?
C32 C33 C34 C35 -2.4(8) . . . . ?
C33 C34 C35 C36 -0.1(4) . . . . ?
C32 C31 C36 C35 -0.6(8) . . . . ?
N5B C31 C36 C35 -4.3(12) . . . . ?
C30 C31 C36 C35 178.1(2) . . . . ?
C32 C31 C36 C37 177.6(7) . . . . ?
N5B C31 C36 C37 173.9(12) . . . . ?
C30 C31 C36 C37 -3.7(4) . . . . ?
C34 C35 C36 C31 1.6(4) . . . . ?
C34 C35 C36 C37 -176.6(3) . . . . ?
C24 N3 C37 C25 0.3(4) . . . . ?
C24 N3 C37 C36 177.3(2) . . . . ?
N2 C25 C37 N3 0.5(4) . . . . ?
C26 C25 C37 N3 178.3(2) . . . . ?
N2 C25 C37 C36 -176.4(2) . . . . ?
C26 C25 C37 C36 1.3(4) . . . . ?
C31 C36 C37 N3 -174.0(2) . . . . ?
C35 C36 C37 N3 4.2(4) . . . . ?
C31 C36 C37 C25 3.1(4) . . . . ?
C35 C36 C37 C25 -178.8(2) . . . . ?
C44 C39 C40 C41 -0.9(5) . . . . ?
C38 C39 C40 C41 179.2(3) . . . . ?
C39 C40 C41 C42 -0.1(5) . . . . ?
C40 C41 C42 C43 1.1(5) . . . . ?
C41 C42 C43 C44 -1.0(5) . . . . ?
C42 C43 C44 C39 0.0(5) . . . . ?
C40 C39 C44 C43 1.0(5) . . . . ?
C38 C39 C44 C43 -179.1(3) . . . . ?
C51 C46 C47 C48 0(3) . . . . ?
C45 C46 C47 C48 177.7(19) . . . . ?
C46 C47 C48 C49 0(3) . . . . ?
C47 C48 C49 C50 0(4) . . . . ?
C48 C49 C50 C51 0(4) . . . . ?
C49 C50 C51 C46 -1(3) . . . . ?
C47 C46 C51 C50 1(3) . . . . ?
C45 C46 C51 C50 -177.0(18) . . . . ?
 
_refine_diff_density_max    0.482
_refine_diff_density_min   -0.592
_refine_diff_density_rms    0.071



#===========================================================================
# start Validation Reply Form
_vrf_RINTA01_mo_CHEM0048_b0ma
;
PROBLEM: The value of Rint is greater than 0.18, Rint given 0.239
RESPONSE: The poor Rint value may be due to the weak data and poor 
crystalinity. Despite the fact that the exposure was set at 60 sec, 
the data is still not good. May be the copper radiation would give 
a better data set instead of Mo. However, the crystal selected was 
already a better of the batch.  There is about 25% of the observed 
reflections could not be indexed using the current cell even with 
cell now, indicative of the poor crystal quality. Unfortunately, 
the crystal was very difficult to be recrystallized for data 
recollection.
;
_vrf_PLAT002_mo_CHEM0048_b0ma
;
PROBLEM:  Number of Distance or Angle Restraints on AtSite         14 Note
RESPONSE: The bond distance and angle restraints are needed for the 
better refinement of the disordered molecules, the toluene solvent.
;
_vrf_PLAT003_mo_CHEM0048_b0ma
;
PROBLEM: Number of Uiso or Uij Restrained non-H Atoms ...          4 Report
RESPONSE: 24 of the restraints were used in 
the anisotropic refinement of the atoms C46, C47, C48 and C50 using isotropic
restraints with s.u. of 0.01 (6 restraints for each atom).
;
_vrf_PLAT171_mo_CHEM0048_b0ma
;
PROBLEM:  The CIF-Embedded .res File Contains EADP Records          1 Report
RESPONSE: The disordered atoms N5/C32B and N5B/C32 is very close in location
and thus assumed very similar anisotropic parameters for stability of 
refinemnet.
;
_vrf_PLAT175_mo_CHEM0048_b0ma
;
PROBLEM: The CIF-Embedded .res File Contains SAME Records          1 Report
RESPONSE: One of the toluene molecule is sitting on the inversion centre,
(0.5, 0, 1), since the toluene molecule does not have inversion centre in the 
molecule, the use of PART -1 is necessary to ensure a proper refinement. The 
use of SAME command so that the bond distances of the two toluene molecules 
may be comparable and the refinement be converged.
;
_vrf_PLAT176_mo_CHEM0048_b0ma
;
PROBLEM: The CIF-Embedded .res File Contains SADI Records          1 Report
RESPONSE: Due to the disorder of the compound molecule, for more stable 
refinemnet, the C---N5(B) or C---C32(B) bond are restrained to be similar to 
those within the molecule using the SADI restraints.
;
_vrf_PLAT213_mo_CHEM0048_b0ma
;
PROBLEM: Atom C32             has ADP max/min Ratio .....        3.3 oblate
RESPONSE: 
;
_vrf_PLAT300_mo_CHEM0048_b0ma
;
PROBLEM: Atom Site Occupancy of *C45 is Constrained at 0.500 Check
Atom Site Occupancy of *C46 is Constrained at 0.500 Check
Atom Site Occupancy of *C47 is Constrained at 0.500 Check
Atom Site Occupancy of *C48 is Constrained at 0.500 Check
Atom Site Occupancy of *C49 is Constrained at 0.500 Check
Atom Site Occupancy of *C50 is Constrained at 0.500 Check
Atom Site Occupancy of *C51 is Constrained at 0.500 Check
Atom Site Occupancy of *H45A is Constrained at 0.500 Check
Atom Site Occupancy of *H45B is Constrained at 0.500 Check
Atom Site Occupancy of *H45C is Constrained at 0.500 Check
Atom Site Occupancy of *H47 is Constrained at 0.500 Check
Atom Site Occupancy of *H48 is Constrained at 0.500 Check
Atom Site Occupancy of *H49 is Constrained at 0.500 Check
Atom Site Occupancy of *H50 is Constrained at 0.500 Check
Atom Site Occupancy of *H51 is Constrained at 0.500 Check
RESPONSE: One of the toluene solvent molecule is disordered on a special 
position of higher symmetry than the toluene molecule can take.
Since the toluene molecule does not have inversion centre, but is sitting on 
the inversion centre, (0.5, 0, 1), the use of PART -1 is necessary to ensure 
the generation of special position constraints is suppressed and bonds to
symmetry generated atoms with the same non-zero PART number are excluded. 
As a result, the site occupancy factor for the whole molecule was set at 0.5. 
;
_vrf_PLAT301_mo_CHEM0048_b0ma
;
PROBLEM: Main Residue  Disorder ............ Percentage =          5 Note
RESPONSE: Due to the close to planar arrangment of the molecule and almost
symmetrical geometry, ignoring the atom N5 and C32, thus, flipping the 
molecule by 180 degree is not much difference, space-wise. As a result, the
molecule may be disordered.
;
_vrf_PLAT302_mo_CHEM0048_b0ma
;
PROBLEM: Anion/Solvent Disorder ............ Percentage =         33 Note
RESPONSE: One of the toluene molecule is disordered.
;
_vrf_PLAT304_mo_CHEM0048_b0ma
;
PROBLEM: Non-Integer Number of Atoms ( 7.50) in Resd. # 3 Check
RESPONSE: One of the toluene solvent molecule is disordered on a special 
position of higher symmetry than the toluene molecule can take.
Since the toluene molecule does not have inversion centre, but is sitting on 
the inversion centre, (0.5, 0, 1), the use of PART -1 is necessary to ensure 
the generation of special position constraints is suppressed and bonds to
symmetry generated atoms with the same non-zero PART number are excluded. 
As a result, the site occupancy factor for the whole molecule 
was set at 0.5. 
;
_vrf_PLAT333_mo_CHEM0048_b0ma
;
PROBLEM: Check Large Av C6-Ring C-C Dist. C9     -C21           1.42 Ang.
Check Large Av C6-Ring C-C Dist. C25    -C37           1.44 Ang.
RESPONSE: This may be related to the poor cyrstal quality of the crystal.
;
_vrf_PLAT340_mo_CHEM0048_b0ma
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0045 Ang.
RESPONSE: This may be related to the poor cyrstal quality of the crystal.
;
_vrf_PLAT411_mo_CHEM0048_b0ma
;
PROBLEM: Short Inter H...H Contact  H27    ..  H27     ..       2.05 Ang
RESPONSE: The molecules are packed very tightly in the unit cell.
;
_vrf_PLAT789_mo_CHEM0048_b0ma
;
PROBLEM: Atoms with Negative _atom_site_disorder_group  #         15 Check
RESPONSE: One of the toluene solvent molecule was siting on the inversion 
centre, (1/2, 0,  1). However, the toluene itself does not have an inversion
symmetry, thus, assignment of negative sign is essential.
;
_vrf_PLAT860_mo_CHEM0048_b0ma
;
PROBLEM: Number of Least-Squares Restraints .............        39 Note
RESPONSE: A total of 49 restraints have been used. 24 of the restraints 
were used in the anisotropic refinement of the atoms C46, C47, C48 and C50 
using isotropic restraints with s.u. of 0.01 (6 restraints for each atom). 
The other 25 restraints were used in restraining the bond distances of 
disordered moiety to be similar to other equivalent parts in the compound 
or equivalent molecule. The crystal quality was not very good, as reflected 
by the big R(int) value obtained.  One EADP constraints was used for N5 and 
C32B. The constraints was needed to prevent non-positive definite of the 
atom N5B/B32B which may be resulted from the poor crystal quality, as 
reflected by the big R(int) value obtained.

;
_vrf_PLAT906_mo_CHEM0048_b0ma
;
PROBLEM: Large K value in the Analysis of Variance ......      4.401 Check
RESPONSE: This may be due to the shape of the crystal resembling a plate and
the poor crystal quality, as reflected from the big R(int) value. 
;
_vrf_PLAT909_mo_CHEM0048_b0ma
;
PROBLEM: Percentage of Observed Data at Theta(Max) still          67 %
RESPONSE: 
;
_vrf_PLAT910_mo_CHEM0048_b0ma
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...          6 Report
RESPONSE: The reflections may be cut by the beam stop.
;
_vrf_PLAT911_mo_CHEM0048_b0ma
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.595          5 Report
RESPONSE: The reflections may be due to missing cusp of data (due to 
rotation about one axis).
;
_vrf_PLAT_mo_CHEM0048_b0ma
;
PROBLEM: 
RESPONSE: 
;
# End Validation Reply Form
#===========================================================================
data_General
_audit_creation_date                  '2015-Nov-10'
_audit_creation_method                'SHELXL'
_audit_update_record                   
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2015-Nov-10 # Formatted by publCIF
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#============================================================================

# PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic     ?
_journal_date_from_coeditor       ?
_journal_date_accepted            ?
_journal_coeditor_code            ?

#============================================================================

# SUBMISSION DETAILS

_publ_contact_author_name             'Professor Wai Kin Chan'
_publ_contact_author_email            'waichan@hku.hk'
_publ_contact_author_fax              '(852)2915 5176'
_publ_contact_author_phone            '(852)2859 8943'
_publ_contact_author_address
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR, 
P. R. CHINA
;
_publ_contact_letter
;
    ENTER TEXT OF LETTER
;
_publ_requested_journal               'ENTER JOURNAL NAME HERE'
_publ_requested_category            ?  #'CHOOSE FI FM FO CI CM CO or AD'
_publ_requested_coeditor_name          ?

#============================================================================

# TITLE AND AUTHOR LIST

_publ_section_title
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Directory Reference: COM774-CHEM0048  D8V_WKC-YuanYuping's 
WKC-Y9.10(2)  31-Jan-2015 // 10-Nov-2015
;
_publ_section_title_footnote .

loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Yuan, Yuping'  .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR, 
P. R. CHINA
;
'Chan, Wai-Kin '   .
;
Department of Chemistry
The University of Hong Kong
Pokfulam Road, Pokfulam,
Hong Kong SAR, 
P. R. CHINA
;

_publ_section_synopsis     .


#============================================================================

# TEXT

_publ_section_abstract  
;
(type here to add abstract)
;

_publ_section_comment
;
The compound 2(C₃₇H₃₅N₅S₂).3(C₇H₈), was
crystallized in a centrosymmetric triclinic space group, P-1 (#2).

The molecule is almost planar. 

;
_publ_section_references
;
Bruker AXS Inc. (2014). APEX2 v2014.11-0, Madison, Wisconsin, USA.

Bruker AXS Inc. (2014). SAINT v.8.34, Madison, Wisconsin, USA.

Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A.
(2008). Mercury. J. Appl. Cryst, 41, 466--470.

Sheldrick, G. M. (2008). SHELX program. SHELXL. Acta Cryst. E64,
112-122.

Sheldrick, G. M. (2014/5). SADABS, Göttingen University, Göttingen,
Germany.

Sheldrick, G. M. (2014/7). SHELX program.
Sheldrick, G. M. (2015). XT program.  Acta Cryst. A71, 3-8.

;
 _publ_section_acknowledgements  
;
The authors thank The University of Hong Kong's University Development Fund and 
the Dr. Hui Wai Haan Fund for funding the purchase of the Bruker D8 Venture 
Photon100 CMOS X-Ray Diffractometer.
;


_publ_section_figure_captions
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Fig. 1. The compound molecule was shown at 50% probability thermal ellipsoids
with the atom numbering scheme.

Fig. 2. The unit cell packing diagram of the compound projected down the
a-axis. 
;

_publ_section_exptl_prep
;
A red block crystal of, 2(C₃₇H₃₅N₅S₂).3(C₇H₈), having approximate 
dimensions of 0.089 mm x 0.222 mm x 0.319 mm was mounted on 
Cryo-loop. All
measurements were made on a Bruker D8 Venture X-ray Diffractometer
equipped with compact optics monochromated microfocus Mo source Kα radiation
and Photon100 CMOS detector.

Cell constants and an orientation matrix for data collection corresponded to a
primitive triclinic cell with dimensions: a =  7.976(3)Å, b =
 11.053(4) Å, c = 22.319(7)Å, V =  1899.8(11)Å³ α = 79.904(9)°
β = 80.498(10)° γ = 82.348(9)°.

For Z = 1 and F.W. = 1504.04, the calculated density is 1.315 g/cm³.
Based on a statistical analysis of intensity distribution, and the successful
solution and refinement of the structure, the space group was determined to
be: P-1 (#2)

The data were collected at a temperature of 100(1)K to a maximum 2θ value
of 50.04°. The crystal-to-detector distance was 50.00 mm. The exposure time
is 60 sec.

Of the 43507 reflections that were collected, 6708 reflections were unique.
(Rint = 0.2361); equivalent reflections were merged.
;
_publ_section_exptl_refinement
;
The structure was solved by XT (Sheldrick, 2015). 
All of the non-H atoms were refined anisotropically.

All of the C-bound H atoms were observable from difference Fourier map but were
all placed at geometrical positions with C---H = 0.95, 0.98 & 0.99Å
for phenyl, methyl and methylene H-atoms respectively. All C-bound
H-atoms were refined using riding model with Uiso(H) =
1.2Ueq(Carrier) for phenyl and methylene H atoms or Uiso(H) = 
1.5Ueq(Carrier) for methyl H atoms. 
A total of 49 restraints have been used. 24 of the restraints were used in 
the anisotropic refinement of the atoms C46, C47, C48 and C50 using isotropic
restraints with s.u. of 0.01 (6 restraints for each atom). The other 25 
restraints were used in restraining the bond distances of disordered moiety to
be similar to other equivalent parts in the compound or equivalent molecule.
The crystal quality was not very good, as reflected by the big R(int) value
obtained. 

Highest peak is  0.48  at  (0.1303, 0.1593, 0.4688)  [  1.06 A from S2 ]
Deepest hole is -0.59  at  (0.0365, 0.4379, 0.3987)  [  0.86 A from S1 ]
;
#===========================================================================