The unexpected and facile molybdenum mediated formation of tri- and tetracyclic pentathiepins from pyrazine-alkynes and sulfur
Muhammad Zubair; Ashta Chandra Ghosh; Carola Schulzke; Chem.Commun. 49 (2013) 4343–; doi:10.1039/c2cc37025e

data_7109218
_publ_section_title
;
 The unexpected and facile molybdenum mediated formation of tri- and
 tetracyclic pentathiepins from pyrazine-alkynes and sulfur
;
_journal_name_full               Chem.Commun.
_journal_page_first              4343
_journal_paper_doi               10.1039/c2cc37025e
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C13 H10 N2 O S5'
_chemical_formula_weight         370.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1317(16)
_cell_length_b                   20.856(4)
_cell_length_c                   8.7162(17)
_cell_measurement_reflns_used    5986
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      31.3407
_cell_measurement_theta_min      1.9515
_cell_volume                     1447.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
scan:
Number of images: 360
Slice: -110.0000 - 70.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 0.0000
XTD: 44.9941
2theta: -19.9523
scan:
Number of images: 280
Slice: -75.0000 - 65.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 90.0000
XTD: 44.9941
2theta: -19.9523
scan:
Number of images: 220
Slice: -55.0000 - 55.0000
Image width: 0.5000
Exp time: 20.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 90.0000
XTD: 44.9941
2theta: -19.9523

;
_diffrn_measurement_device
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15450
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.39
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.8010
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0444
_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/[\s^2^(Fo^2^)+(0.1103P)^2^+1.3760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                4112
_reflns_number_total             4250
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc37025e.txt
_cod_data_source_block           mz4
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7109218