Pd-Catalyzed One-Pot Sequential Cross-Coupling Reactions of Tetrabromothiophene
Saini, Kapil Mohan; Saunthwal, Rakesh K.; Verma, Akhilesh K.; Organic & Biomolecular Chemistry  (2017) –; doi:10.1039/C7OB02601C

data_7155989
_publ_section_title
;
 Pd-Catalyzed One-Pot Sequential Cross-Coupling Reactions of
 Tetrabromothiophene
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/C7OB02601C
_journal_year                    2017
_chemical_formula_moiety         'C36 H28 S'
_chemical_formula_sum            'C36 H28 S'
_chemical_formula_weight         492.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-09-27 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                111.486(10)
_cell_angle_beta                 93.777(7)
_cell_angle_gamma                100.958(8)
_cell_formula_units_Z            2
_cell_length_a                   9.4120(7)
_cell_length_b                   12.0734(14)
_cell_length_c                   13.3979(14)
_cell_measurement_reflns_used    4817
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.12
_cell_volume                     1375.5(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Supernova (Mo) X-ray source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9019
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.103
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Crysalispro
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1832P)^2^+0.0605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2601
_refine_ls_wR_factor_ref         0.2968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3275
_reflns_number_total             4817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob02601c2.cif
_cod_data_source_block           shelx
_cod_database_code               7155989
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              52197