Organoselenium-catalyzed vicinal dichlorination of unsaturated phosphonates
Zeng, Xianghua; Gong, Chunhua; Zhang, Junyong; Xie, Jingli; New J. Chem. 40 (2016) 7866–; doi:10.1039/C6NJ00658B

data_7055693
_publ_section_title
;
 Organoselenium-catalyzed vicinal dichlorination of unsaturated
 phosphonates
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7866
_journal_paper_doi               10.1039/C6NJ00658B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C12 H10 Cl2 Se'
_chemical_formula_weight         304.06
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.7839(6)
_cell_length_b                   7.6076(3)
_cell_length_c                   17.9304(12)
_cell_measurement_reflns_used    1926
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      72.0840
_cell_measurement_theta_min      4.9920
_cell_volume                     2425.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.739
_diffrn_measured_fraction_theta_max 0.740
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4198
_diffrn_reflns_theta_full        72.18
_diffrn_reflns_theta_max         72.18
_diffrn_reflns_theta_min         4.97
_exptl_absorpt_coefficient_mu    7.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16971
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.426
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                1578
_reflns_number_total             1766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj00658b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7055693--7055694.cif.'
_cod_original_cell_volume        2425.86(19)
_cod_database_code               7055693