3,4-Dibromo-2,5-bis[(diethoxyphosphoryl)methyl]-1-phenylsulfonyl-1<i>H</i>-pyrrole
Karthikeyan, S.; Sethusankar, K.; Rajeswaran, Ganesan Gobi; Mohanakrishnan, Arasambattu K.; Acta Crystallographica Section E 67 (2011) o2212–o2213; doi:10.1107/S1600536811030273

data_2231661
_publ_section_title
;
 3,4-Dibromo-2,5-bis[(diethoxyphosphoryl)methyl]-1-phenylsulfonyl-1<i>H</i>-pyrrole
;
_journal_coeditor_code           PV2427
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2212
_journal_page_last               o2213
_journal_paper_doi               10.1107/S1600536811030273
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H29 Br2 N O8 P2 S'
_chemical_formula_moiety         'C20 H29 Br2 N O8 P2 S'
_chemical_formula_sum            'C20 H29 Br2 N O8 P2 S'
_chemical_formula_weight         665.26
_chemical_name_common
;
3,4-Dibromo-2,5-bis[(diethoxyphosphoryl)methyl]-1-phenylsulfonyl-
1<i>H</i>-pyrrole
;
_chemical_name_systematic
;
diethyl {[1-(benzenesulfonyl)-3,4-dibromo-5-
[(diethoxyphosphoryl)methyl]-1<i>H</i>-pyrrol-2-yl]methyl}phosphonate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.5060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6524(2)
_cell_length_b                   17.5137(5)
_cell_length_c                   15.8965(4)
_cell_measurement_reflns_used    8138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.33
_cell_volume                     2674.89(12)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       \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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34672
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.272
_exptl_absorpt_correction_T_max  0.5607
_exptl_absorpt_correction_T_min  0.4402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.763
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8138
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1.4803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                4819
_reflns_number_total             8138
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2427.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231661
_cod_database_fobs_code          2231661