Reactions of Nitrosoalkenes with Dipyrromethanes and Pyrroles: Insight into the Mechanistic Pathway.
Nunes, Sandra C. C.; Lopes, Susana M. M.; Gomes, Clara S. B.; Lemos, Américo; Pais, Alberto A. C. C.; Pinho E Melo, Teresa M V D; The Journal of organic chemistry 79 (2014) 10456–; doi:10.1021/jo502095k

data_4030087
_publ_section_title
;
 Reactions of Nitrosoalkenes with Dipyrromethanes and Pyrroles: Insight
 into the Mechanistic Pathway.
;
_journal_issue                   21
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10456
_journal_paper_doi               10.1021/jo502095k
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C14 H15 Br N2 O, H2 O'
_chemical_formula_sum            'C14 H17 Br N2 O2'
_chemical_formula_weight         325.21
_chemical_name_systematic
;     
2-(4-bromophenyl)-3a,5-dimethyl-
-3,3a,6,6a-tetrahydropyrrolo[3,2-b]pyrrole 1-oxide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 95.621(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5819(12)
_cell_length_b                   11.1103(17)
_cell_length_c                   16.530(3)
_cell_measurement_reflns_used    775
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.01
_cell_measurement_theta_min      3.08
_cell_volume                     1385.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1365
_diffrn_reflns_av_sigmaI/netI    0.1375
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11044
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_T_max  0.7558
_exptl_absorpt_correction_T_min  0.3833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                1418
_reflns_number_total             2584
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo502095k_si_002.cif
_cod_data_source_block           18
_cod_depositor_comments
'Adding full bibliography for 4030086--4030087.cif.'
_cod_original_cell_volume        1385.8(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4030087