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_7042397
_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 H15 Co N2 O S2'
_chemical_formula_sum            'C18 H15 Co N2 O S2'
_chemical_formula_weight         398.37
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3368 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.169(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.1653(2)
_cell_length_b                   19.6347(6)
_cell_length_c                   16.9400(5)
_cell_measurement_reflns_used    20591
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.8350
_cell_measurement_theta_min      3.8590
_cell_volume                     3367.35(16)
_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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'HPAD Dectris Pilatus200K'
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9202
_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     56.00  88.00   0.50    9.09    --   -0.30  38.00-150.00   64
  2  \w    -23.00  28.00   0.50    9.09    --   -0.30  38.00 -90.00  102
  3  \w    -19.00  89.00   0.50    9.09    --   -0.30  19.00 120.00  216
  4  \w     -7.00  73.00   0.50    9.09    --   -0.30  38.00 -60.00  160
  5  \w     27.00  87.00   0.50    9.09    --   -0.30  38.00-180.00  120
  6  \w     37.00  74.00   0.50    9.09    --   -0.30  38.00 -30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0346479000
_diffrn_orient_matrix_UB_12      -0.0270376000
_diffrn_orient_matrix_UB_13      0.0166315000
_diffrn_orient_matrix_UB_21      -0.0608417000
_diffrn_orient_matrix_UB_22      0.0151042000
_diffrn_orient_matrix_UB_23      -0.0143856000
_diffrn_orient_matrix_UB_31      0.0009964000
_diffrn_orient_matrix_UB_32      -0.0186253000
_diffrn_orient_matrix_UB_33      -0.0358370000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54264
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.742
_diffrn_reflns_theta_min         3.649
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Rigaku mm003 (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55077
_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    1.572
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile / water'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.0027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8636
_reflns_number_total             9670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00377c2.cif
_cod_data_source_block           TF343
_cod_depositor_comments
'Adding full bibliography for 7042394--7042397.cif.'
_cod_original_cell_volume        3367.36(16)
_cod_database_code               7042397
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3'B(H3'B), C1'B(H1'B), C2'B(H2'B), C4(H4), C4'B(H4'B), C6(H6),
 C5'B(H5'B), C5'(H5'), C5(H5), C4B(H4B), C3'(H3'), C5B(H5B), C2'(H2'), C1'(H1'),
  C4'(H4'), C7B(H7B), C6B(H6B)
2.b Idealised Me refined as rotating group:
 C13B(H13D,H13E,H13F), C12B(H12D,H12E,H12F), C13(H13A,H13B,H13C), C12(H12A,
 H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.138
_oxdiff_exptl_absorpt_empirical_full_min 0.706