First reductive dimerization of a polycyclic azine
Berthet, Jean-Claude; Thuéry, Pierre; Baudin, Cécile; Boizot, Bruno; Ephritikhine, Michel; Dalton Transactions  (2009) 7613–7616; doi:10.1039/b909547k

data_7002277
_publ_section_title
;
 First reductive dimerization of a polycyclic azine
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7613
_journal_page_last               7616
_journal_paper_doi               10.1039/b909547k
_journal_year                    2009
_chemical_formula_sum            'C44 H36 I6 N16 U2'
_chemical_formula_weight         2026.35
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.106(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.314(2)
_cell_length_b                   13.4164(9)
_cell_length_c                   16.0957(10)
_cell_measurement_reflns_used    18972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.13
_cell_volume                     5466.5(7)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       '\f scan with 2\% steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1511
_diffrn_reflns_av_sigmaI/netI    0.1241
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18972
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.353
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.255
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DELABS (PLATON, 2003)'
_exptl_crystal_colour            'translucent light brown'
_exptl_crystal_density_diffrn    2.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5005
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+86.3501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.2138
_reflns_number_gt                2618
_reflns_number_total             5005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909547k.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7002277