 
data_90mz09
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C48 H30 N12 S6'
_chemical_formula_weight          967.20
 
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'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    8.6400(10)
_cell_length_b                    9.940(3)
_cell_length_c                    14.473(5)
_cell_angle_alpha                 72.98(5)
_cell_angle_beta                  80.27(2)
_cell_angle_gamma                 73.73(3)
_cell_volume                      1135.8(5)
_cell_formula_units_Z             1
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.2
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.414
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              498
_exptl_absorpt_coefficient_mu     0.352
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'ENRAF NOnius CAD4'
_diffrn_measurement_method        'Sequential collection'
_diffrn_detector_area_resol_mean  'n/a'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             2385
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0040
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          25.02
_reflns_number_total              2385
_reflns_number_gt                 2385
_reflns_threshold_expression      >2σ(I)
 

_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.1309P)²+0.8610P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2385
_refine_ls_number_parameters      298
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0593
_refine_ls_R_factor_gt            0.0593
_refine_ls_wR_factor_ref          0.2185
_refine_ls_wR_factor_gt           0.2185
_refine_ls_goodness_of_fit_ref    1.504
_refine_ls_restrained_S_all       1.504
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S3 S 0.91345(19) 0.86104(19) 0.14390(13) 0.0503(5) Uani 1 1 d . . .
S2 S 0.7079(2) 0.9334(2) -0.01630(15) 0.0627(6) Uani 1 1 d . . .
S1 S 1.04384(17) 0.73890(18) -0.01606(11) 0.0434(5) Uani 1 1 d . . .
C4 C 1.1927(8) 0.7345(8) 0.2374(5) 0.0545(18) Uani 1 1 d . . .
H4A H 1.1937 0.6405 0.2808 0.082 Uiso 1 1 calc R . .
H4B H 1.1368 0.8080 0.2703 0.082 Uiso 1 1 calc R . .
H4C H 1.3020 0.7429 0.2168 0.082 Uiso 1 1 calc R . .
C1 C 1.3353(7) 0.5971(8) 0.0649(5) 0.0547(18) Uani 1 1 d . . .
H1A H 1.4153 0.6520 0.0534 0.082 Uiso 1 1 calc R . .
H1B H 1.3434 0.5565 0.0112 0.082 Uiso 1 1 calc R . .
H1C H 1.3533 0.5204 0.1233 0.082 Uiso 1 1 calc R . .
C7 C 0.7951(8) 0.5010(7) 0.1738(5) 0.0412(14) Uani 1 1 d . . .
C22 C 0.6104(6) 0.0391(5) 0.4187(4) 0.0292(11) Uani 1 1 d . . .
C19 C 0.6693(7) 0.1461(7) 0.2434(5) 0.0418(14) Uani 1 1 d . . .
C23 C 0.4416(6) 0.0694(6) 0.4095(4) 0.0295(12) Uani 1 1 d . . .
H23 H 0.4030 0.1161 0.3491 0.035 Uiso 1 1 calc R . .
C15 C 0.7804(6) 0.3242(6) 0.4435(4) 0.0337(12) Uani 1 1 d . . .
H15 H 0.8891 0.3029 0.4534 0.040 Uiso 1 1 calc R . .
C10 C 0.7310(6) 0.3932(6) 0.3483(4) 0.0312(12) Uani 1 1 d . . .
C13 C 0.5029(6) 0.3196(6) 0.5080(4) 0.0302(12) Uani 1 1 d . . .
C14 C 0.6711(7) 0.2893(6) 0.5198(4) 0.0334(12) Uani 1 1 d . . .
H14 H 0.7065 0.2445 0.5811 0.040 Uiso 1 1 calc R . .
C24 C 0.3361(6) 0.0312(6) 0.4876(4) 0.0308(12) Uani 1 1 d . . .
H24 H 0.2267 0.0515 0.4795 0.037 Uiso 1 1 calc R . .
C11 C 0.5627(6) 0.4225(6) 0.3361(4) 0.0325(12) Uani 1 1 d . . .
H11 H 0.5277 0.4660 0.2745 0.039 Uiso 1 1 calc R . .
N2 N 1.1494(7) 0.3791(8) 0.2825(5) 0.0633(17) Uani 1 1 d . . .
N1 N 0.7586(8) 0.5571(7) 0.0974(4) 0.0585(16) Uani 1 1 d . . .
C16 C 0.3903(6) 0.2843(6) 0.5865(4) 0.0331(12) Uani 1 1 d . . .
C18 C 0.4353(7) 0.2174(7) 0.6830(4) 0.0377(13) Uani 1 1 d . . .
N5 N 0.6305(8) 0.1999(7) 0.1658(4) 0.0645(17) Uani 1 1 d . . .
C9 C 1.0121(8) 0.4014(7) 0.2781(4) 0.0431(15) Uani 1 1 d . . .
C12 C 0.4538(6) 0.3884(6) 0.4118(4) 0.0324(12) Uani 1 1 d . . .
H12 H 0.3451 0.4097 0.4017 0.039 Uiso 1 1 calc R . .
C8 C 0.8438(7) 0.4317(6) 0.2698(4) 0.0366(13) Uani 1 1 d . . .
C20 C 0.7204(7) 0.0783(6) 0.3377(4) 0.0346(13) Uani 1 1 d . . .
C2 C 1.1705(7) 0.6943(7) 0.0754(4) 0.0397(14) Uani 1 1 d . . .
N6 N 1.0263(7) 0.0265(7) 0.3458(5) 0.0628(17) Uani 1 1 d . . .
C3 C 1.1075(7) 0.7537(6) 0.1502(4) 0.0403(14) Uani 1 1 d . . .
C6 C 0.7300(10) 0.8573(10) -0.1166(6) 0.075(2) Uani 1 1 d . . .
H6D H 0.8239 0.8767 -0.1589 0.113 Uiso 1 1 calc R . .
H6E H 0.6356 0.9000 -0.1516 0.113 Uiso 1 1 calc R . .
H6F H 0.7423 0.7544 -0.0933 0.113 Uiso 1 1 calc R . .
C5 C 0.8851(7) 0.8453(6) 0.0347(5) 0.0415(15) Uani 1 1 d . . .
C21 C 0.8884(7) 0.0496(7) 0.3437(4) 0.0410(14) Uani 1 1 d . . .
C17 C 0.2215(7) 0.3132(6) 0.5770(4) 0.0364(13) Uani 1 1 d . . .
N3 N 0.0854(7) 0.3338(7) 0.5721(4) 0.0575(15) Uani 1 1 d . . .
N4 N 0.4660(7) 0.1640(7) 0.7610(4) 0.0545(15) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
S3 C5 1.696(7) . ?
S3 C3 1.717(6) . ?
S2 C5 1.705(6) . ?
S2 C6 1.784(9) . ?
S1 C5 1.686(6) . ?
S1 C2 1.739(6) . ?
C4 C3 1.506(9) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C1 C2 1.492(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C7 N1 1.137(8) . ?
C7 C8 1.433(8) . ?
C22 C20 1.411(7) . ?
C22 C24 1.420(7) 2_656 ?
C22 C23 1.425(7) . ?
C19 N5 1.155(8) . ?
C19 C20 1.418(9) . ?
C23 C24 1.359(7) . ?
C23 H23 0.9300 . ?
C15 C14 1.355(8) . ?
C15 C10 1.426(8) . ?
C15 H15 0.9300 . ?
C10 C8 1.402(8) . ?
C10 C11 1.432(8) . ?
C13 C16 1.394(8) . ?
C13 C14 1.429(7) . ?
C13 C12 1.438(7) . ?
C14 H14 0.9300 . ?
C24 C22 1.420(7) 2_656 ?
C24 H24 0.9300 . ?
C11 C12 1.347(8) . ?
C11 H11 0.9300 . ?
N2 C9 1.154(8) . ?
C16 C18 1.428(8) . ?
C16 C17 1.428(8) . ?
C18 N4 1.139(8) . ?
C9 C8 1.419(8) . ?
C12 H12 0.9300 . ?
C20 C21 1.411(8) . ?
C2 C3 1.345(8) . ?
N6 C21 1.152(8) . ?
C6 H6D 0.9600 . ?
C6 H6E 0.9600 . ?
C6 H6F 0.9600 . ?
C17 N3 1.146(8) . ?
 
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 S3 C3 96.9(3) . . ?
C5 S2 C6 102.0(3) . . ?
C5 S1 C2 97.0(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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 . . ?
N1 C7 C8 178.8(7) . . ?
C20 C22 C24 121.2(5) . 2_656 ?
C20 C22 C23 121.2(5) . . ?
C24 C22 C23 117.6(5) 2_656 . ?
N5 C19 C20 178.6(7) . . ?
C24 C23 C22 121.1(5) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C14 C15 C10 121.0(5) . . ?
C14 C15 H15 119.5 . . ?
C10 C15 H15 119.5 . . ?
C8 C10 C15 120.9(5) . . ?
C8 C10 C11 121.5(5) . . ?
C15 C10 C11 117.7(5) . . ?
C16 C13 C14 121.5(5) . . ?
C16 C13 C12 121.2(5) . . ?
C14 C13 C12 117.3(5) . . ?
C15 C14 C13 121.5(5) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C23 C24 C22 121.3(5) . 2_656 ?
C23 C24 H24 119.3 . . ?
C22 C24 H24 119.3 2_656 . ?
C12 C11 C10 121.5(5) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C16 C18 122.4(5) . . ?
C13 C16 C17 122.8(5) . . ?
C18 C16 C17 114.9(5) . . ?
N4 C18 C16 177.7(6) . . ?
N2 C9 C8 178.3(7) . . ?
C11 C12 C13 121.1(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C10 C8 C9 123.3(5) . . ?
C10 C8 C7 121.2(5) . . ?
C9 C8 C7 115.4(5) . . ?
C21 C20 C22 122.9(5) . . ?
C21 C20 C19 115.2(5) . . ?
C22 C20 C19 121.8(5) . . ?
C3 C2 C1 126.2(6) . . ?
C3 C2 S1 115.0(4) . . ?
C1 C2 S1 118.7(5) . . ?
C2 C3 C4 125.6(5) . . ?
C2 C3 S3 116.4(5) . . ?
C4 C3 S3 118.0(4) . . ?
S2 C6 H6D 109.5 . . ?
S2 C6 H6E 109.5 . . ?
H6D C6 H6E 109.5 . . ?
S2 C6 H6F 109.5 . . ?
H6D C6 H6F 109.5 . . ?
H6E C6 H6F 109.5 . . ?
S1 C5 S3 114.6(3) . . ?
S1 C5 S2 124.6(4) . . ?
S3 C5 S2 120.8(3) . . ?
N6 C21 C20 178.0(7) . . ?
N3 C17 C16 177.9(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.593
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.593
_refine_diff_density_max    0.555
_refine_diff_density_min   -0.394
_refine_diff_density_rms    0.104
