#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:18:07 +0100 (lun 21 de mar de 2016) $
#$Revision: 178379 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/01/4020118.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4020118
loop_
_publ_author_name
'Shigehisa Akine'
'Takanori Taniguchi'
'Wenkui Dong'
'Sayuri Masubuchi'
'Tatsuya Nabeshima'
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1704
_journal_page_last               1711
_journal_paper_doi               10.1021/jo048030y
_journal_volume                  70
_journal_year                    2005
_chemical_formula_moiety         C18H20N2O6
_chemical_formula_sum            'C18 H20 N2 O6'
_chemical_formula_weight         360.36
_chemical_melting_point          386
_chemical_name_common            H2(3-MeOsalamo)
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.065(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.694(4)
_cell_length_b                   14.616(6)
_cell_length_c                   12.356(4)
_cell_measurement_reflns_used    5122
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.79
_cell_volume                     839.3(9)
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD system'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2079
_diffrn_reflns_av_sigmaI/netI    0.1960
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5122
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.9380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.2089
_refine_ls_R_factor_gt           0.0816
_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/[σ²(Fo²)+(0.0959P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.2330
_reflns_number_gt                614
_reflns_number_total             1482
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4020118
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2631(12) 0.2441(4) 0.0856(4) 0.0229(14) Uani 1 1 d . . .
C2 C 0.1586(13) 0.2152(4) -0.0202(4) 0.0254(15) Uani 1 1 d . . .
C3 C -0.0509(13) 0.1484(4) -0.0366(4) 0.0238(15) Uani 1 1 d . . .
C4 C -0.1634(13) 0.1088(4) 0.0501(4) 0.0280(15) Uani 1 1 d . . .
H1 H -0.3057 0.0623 0.0379 0.034 Uiso 1 1 calc R . .
C5 C -0.0611(14) 0.1392(4) 0.1576(4) 0.0295(16) Uani 1 1 d . . .
H2 H -0.1359 0.1136 0.2184 0.035 Uiso 1 1 calc R . .
C6 C 0.1471(13) 0.2061(4) 0.1732(4) 0.0264(15) Uani 1 1 d . . .
H3 H 0.2133 0.2267 0.2453 0.032 Uiso 1 1 calc R . .
O1 O 0.2541(9) 0.2509(3) -0.1109(3) 0.0330(12) Uani 1 1 d . . .
H4 H 0.3803 0.2907 -0.0918 0.050 Uiso 1 1 calc R . .
O2 O -0.1340(9) 0.1234(3) -0.1448(3) 0.0304(11) Uani 1 1 d . . .
C7 C -0.3786(15) 0.0622(4) -0.1684(5) 0.0365(17) Uani 1 1 d . . .
H5 H -0.3281 0.0019 -0.1368 0.055 Uiso 1 1 calc R . .
H6 H -0.4306 0.0564 -0.2478 0.055 Uiso 1 1 calc R . .
H7 H -0.5423 0.0871 -0.1367 0.055 Uiso 1 1 calc R . .
C8 C 0.4803(14) 0.3156(4) 0.1069(4) 0.0288(16) Uani 1 1 d . . .
H8 H 0.5467 0.3331 0.1802 0.035 Uiso 1 1 calc R . .
N1 N 0.5831(11) 0.3553(3) 0.0282(4) 0.0258(12) Uani 1 1 d . . .
O3 O 0.7862(9) 0.4230(3) 0.0669(3) 0.0322(12) Uani 1 1 d . . .
C9 C 0.8991(14) 0.4635(4) -0.0240(4) 0.0285(15) Uani 1 1 d . . .
H9 H 0.7423 0.4900 -0.0766 0.034 Uiso 1 1 calc R . .
H10 H 1.0023 0.4172 -0.0624 0.034 Uiso 1 1 calc R . .
