Diethyl 3-amino-4-[(triphenylphosphoranylidene)amino]thieno[2,3-<i>b</i>]thiophene-2,5-dicarboxylate
Wang, Xiang; Li, Yan; Liu, Ming-Guo; Acta Crystallographica Section E 64 (2008) o1180–; doi:10.1107/S1600536808015705

data_2218609
_publ_section_title
;Diethyl
 3-amino-4-[(triphenylphosphoranylidene)amino]thieno[2,3-<i>b</i>]thiophene-2,5-dicarboxylate
;
_journal_coeditor_code           BT2711
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1180
_journal_paper_doi               10.1107/S1600536808015705
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C30 H27 N2 O4 P S2'
_chemical_formula_moiety         'C30 H27 N2 O4 P S2'
_chemical_formula_sum            'C30 H27 N2 O4 P S2'
_chemical_formula_weight         574.63
_chemical_name_systematic
;
Diethyl
3-amino-4-[(triphenylphosphoranylidene)amino]thieno[2,3-<i>b</i>]thiophene-
2,5-dicarboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                68.1400(10)
_cell_angle_beta                 71.0430(10)
_cell_angle_gamma                68.9690(10)
_cell_formula_units_Z            4
_cell_length_a                   13.1260(9)
_cell_length_b                   15.3616(10)
_cell_length_c                   16.6497(11)
_cell_measurement_reflns_used    2577
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.74
_cell_measurement_theta_min      2.28
_cell_volume                     2836.5(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART 4K CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20968
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         10981
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                6314
_reflns_number_total             10981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2711.cif
_cod_data_source_block           I
_cod_database_code               2218609
_cod_database_fobs_code          2218609