Cyclobutane-Derived Diamines: Synthesis and Molecular Structure
Dmytro S. Radchenko; Sergiy O. Pavlenko; Oleksandr O. Grygorenko; Dmitriy M. Volochnyuk; Svitlana V. Shishkina; Oleg V. Shishkin; Igor V. Komarov; Journal of Organic Chemistry 75 (2010) 5941–5952; doi:10.1021/jo101271h

data_4025656
_publ_contact_author
;
  Shishkina S.V.
  Institute for Single Crystals
  60 Lenina ave.
  Kharkiv, 61072
  Ukraine
;
_publ_contact_author_email       sveta@xray.isc.kharkov.com
_publ_contact_author_fax         '380 57 341 02 73'
_publ_contact_author_phone       '380 57 341 02 58'
_publ_section_title
;
 Cyclobutane-Derived Diamines: Synthesis and Molecular Structure
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5941
_journal_page_last               5952
_journal_paper_doi               10.1021/jo101271h
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C16 H21 N3 O5'
_chemical_formula_sum            'C16 H21 N3 O5'
_chemical_formula_weight         335.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.58(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.128(3)
_cell_length_b                   5.9797(11)
_cell_length_c                   19.539(4)
_cell_measurement_reflns_used    3009
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.2
_cell_measurement_theta_min      3.1
_cell_volume                     1685.0(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_molecular_graphics    'XP (Siemens, 1998)'
_computing_publication_material  'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  Xcalibur"3
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16902
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.58
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.111
_refine_diff_density_min         -0.122
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.640
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.640
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                1482
_reflns_number_total             4860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo101271h_si_005.cif
_cod_data_source_block           38
_cod_original_cell_volume        1684.9(5)
_cod_database_code               4025656