The unusual ring scission of a quinoxaline-pyran-fused dithiolene system related to molybdopterin.
Fogeron, Thibault; Retailleau, Pascal; Chamoreau, Lise-Marie; Fontecave, Marc; Li, Yun; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4161–4164; doi:10.1039/c7dt00377c

data_7042395
_publ_section_title
;
 The unusual ring scission of a quinoxaline-pyran-fused dithiolene system
 related to molybdopterin.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4161
_journal_page_last               4164
_journal_paper_doi               10.1039/c7dt00377c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C18 H19 Co N2 O S2'
_chemical_formula_sum            'C18 H19 Co N2 O S2'
_chemical_formula_weight         402.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.08(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.498(4)
_cell_length_b                   5.5628(14)
_cell_length_c                   17.846(5)
_cell_measurement_reflns_used    1883
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.6070
_cell_measurement_theta_min      3.8090
_cell_volume                     1719.8(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXLT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'Dectris HPAD Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      7.00  80.00   0.50   45.00    --    4.40  38.00 -60.00  146
  2  \w    -63.00 -37.00   0.50   45.00    --    4.40 -57.00-180.00   52
  3  \w    -31.00  -5.00   0.50   45.00    --    4.40  57.00 -90.00   52
  4  \w    -75.00 -24.00   0.50   45.00    --   -5.10 -77.00 -30.00  102
  5  \w    -94.00 -45.00   0.50   45.00    --   -5.10 -38.00 -60.00   98
  6  \w    -42.00  83.00   0.50   45.00    --   -5.10 -19.00 120.00  250
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku mm003 XtaLAB Pro: Kappa '
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0410118000
_diffrn_orient_matrix_UB_12      -0.0068884000
_diffrn_orient_matrix_UB_13      -0.0050919000
_diffrn_orient_matrix_UB_21      -0.0013696000
_diffrn_orient_matrix_UB_22      0.0485326000
_diffrn_orient_matrix_UB_23      -0.0370605000
_diffrn_orient_matrix_UB_31      0.0017909000
_diffrn_orient_matrix_UB_32      -0.1182084000
_diffrn_orient_matrix_UB_33      -0.0149071000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1247
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13572
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.349
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.518
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  1.689
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile / water'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3131
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2033
_reflns_number_total             3131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00377c2.cif
_cod_data_source_block           TF369
_cod_depositor_comments
'Adding full bibliography for 7042394--7042397.cif.'
_cod_original_cell_volume        1719.9(7)
_cod_database_code               7042395
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              5569