Reactions of Fused Polycyclic 1,2-Dithiins with Transition Metals: Synthesis of Heteroacenes via Desulfurization
Kudoh, Kenichi; Okamoto, Toshihiro; Yamaguchi, Shigehiro; Organometallics 25 (2006) 2374–; doi:10.1021/om051000g

data_4074915
_publ_section_title
;
 Reactions of Fused Polycyclic 1,2-Dithiins with Transition
 Metals:&#x00A0; Synthesis of Heteroacenes via Desulfurization
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2374
_journal_paper_doi               10.1021/om051000g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C43 H49 Cl2 Ni P S6 Si2'
_chemical_formula_weight         974.94
_chemical_name_common            Nickel-Complex
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(13)
_cell_angle_beta                 101.8198(15)
_cell_angle_gamma                90.0000(13)
_cell_formula_units_Z            4
_cell_length_a                   13.722(4)
_cell_length_b                   21.866(6)
_cell_length_c                   16.436(5)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0677
_cell_volume                     4827(2)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38184
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         10889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.9179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                9240
_reflns_number_total             10889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051000gsi20051120_092316.cif
_cod_data_source_block           Nickel_complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4074915