E versus Z Diazeniumdiolation of Acetoacetate-Derived Carbanions
Navamoney Arulsamy; D. Scott Bohle; Carla L. Holman; Inna Perepichka; Journal of Organic Chemistry 77 (2012) 7313–7318; doi:10.1021/jo301025k

data_4027425
_publ_section_title
;
 E versus Z Diazeniumdiolation of Acetoacetate-Derived Carbanions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7313
_journal_page_last               7318
_journal_paper_doi               10.1021/jo301025k
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C5 H6 N2 O5, 2(C4 H12 N), C H4 O, 3(H2 O)'
_chemical_formula_sum            'C14 H40 N4 O9'
_chemical_formula_weight         408.50
_chemical_name_systematic
; 
 Bis(tetramethylammonium) Methylbutenoate-2-hydroxylate-3-diazeniumdiolate
trihydrate methanolate 
;
_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                 92.384(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6034(1)
_cell_length_b                   8.8273(1)
_cell_length_c                   29.7562(3)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.98
_cell_measurement_theta_min      2.41
_cell_volume                     2257.87(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            37041
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                5691
_reflns_number_total             9014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301025k_si_001.cif
_cod_data_source_block           na36a
_cod_database_code               4027425