#------------------------------------------------------------------------------
#$Date: 2016-03-21 02:17:07 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178378 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/00/4020048.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_4020048
loop_
_publ_author_name
'Kay M. Brummond'
'Sang-phyo Hong'
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              907
_journal_page_last               916
_journal_paper_doi               10.1021/jo0483567
_journal_volume                  70
_journal_year                    2005
_chemical_formula_sum            'C23 H33 N O7'
_chemical_formula_weight         435.50
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1470(10)
_cell_length_b                   24.654(3)
_cell_length_c                   10.642(2)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      7.0
_cell_volume                     2331.5(6)
_diffrn_ambient_temperature      293(2)
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4334
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.091
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_F_000             936
_refine_ls_extinction_coef       0.0076(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0582P)²+0.2217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1382
_refine_ls_wR_factor_obs         0.1099
_reflns_number_observed          2353
_reflns_number_total             4066
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.2217P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.2217P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4020048
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N N 0.4643(2) 0.41904(7) 0.0641(2) 0.0406(5) Uani 1 d . .
H0A H 0.5107(2) 0.44290(7) 0.0291(2) 0.049 Uiso 1 calc R .
O1 O 0.2764(2) 0.50650(6) -0.0606(2) 0.0579(5) Uani 1 d . .
H1A H 0.2170(15) 0.5232(5) -0.1172(20) 0.069 Uiso 1 calc R .
O2 O 0.0531(2) 0.48820(8) -0.2869(2) 0.0697(6) Uani 1 d . .
O3 O 0.1177(2) 0.27255(8) -0.2485(2) 0.0768(7) Uani 1 d . .
O4 O 0.3102(2) 0.32366(8) -0.2832(2) 0.0650(6) Uani 1 d . .
O5 O 0.7270(2) 0.40289(9) 0.6607(2) 0.0757(6) Uani 1 d . .
O6 O 0.4688(2) 0.33074(7) 0.1248(2) 0.0612(5) Uani 1 d . .
O7 O 0.6809(2) 0.37603(7) 0.1099(2) 0.0546(5) Uani 1 d . .
C1 C 0.3139(3) 0.43115(9) 0.0800(2) 0.0421(6) Uani 1 d . .
H1B H 0.2686(3) 0.39695(9) 0.0985(2) 0.051 Uiso 1 calc R .
C2 C 0.2150(3) 0.45429(9) -0.0430(2) 0.0435(6) Uani 1 d . .
H2A H 0.1130(3) 0.45917(9) -0.0306(2) 0.052 Uiso 1 calc R .
C3 C 0.2068(3) 0.41921(9) -0.1619(2) 0.0429(6) Uani 1 d . .
H3A H 0.3094(3) 0.41732(9) -0.1745(2) 0.051 Uiso 1 calc R .
C4 C 0.1105(3) 0.44371(11) -0.2846(3) 0.0512(7) Uani 1 d . .
C5 C 0.0959(3) 0.41017(13) -0.4044(3) 0.0705(9) Uani 1 d . .
H5A H 0.1893(3) 0.41230(13) -0.4322(3) 0.085 Uiso 1 calc R .
H5B H 0.0170(3) 0.42543(13) -0.4725(3) 0.085 Uiso 1 calc R .
C6 C 0.0600(3) 0.35075(12) -0.3863(3) 0.0709(9) Uani 1 d . .
H6A H -0.0440(3) 0.34757(12) -0.3808(3) 0.085 Uiso 1 calc R .
H6B H 0.0716(3) 0.33023(12) -0.4611(3) 0.085 Uiso 1 calc R .
C7 C 0.1608(3) 0.32701(11) -0.2663(3) 0.0556(7) Uani 1 d . .
C8 C 0.1579(3) 0.36074(10) -0.1478(3) 0.0524(7) Uani 1 d . .
H8A H 0.2244(3) 0.34452(10) -0.0725(3) 0.063 Uiso 1 calc R .
H8B H 0.0568(3) 0.36064(10) -0.1340(3) 0.063 Uiso 1 calc R .
C9 C 0.2495(4) 0.24246(14) -0.2042(5) 0.126(2) Uani 1 d . .
H9A H 0.2460(4) 0.20942(14) -0.2543(5) 0.151 Uiso 1 calc R .
H9B H 0.2608(4) 0.23272(14) -0.1141(5) 0.151 Uiso 1 calc R .
C10 C 0.3743(4) 0.27625(13) -0.2190(4) 0.0950(12) Uani 1 d . .
H10A H 0.4384(4) 0.28517(13) -0.1351(4) 0.114 Uiso 1 calc R .
H10B H 0.4343(4) 0.25757(13) -0.2695(4) 0.114 Uiso 1 calc R .
C11 C 0.3225(3) 0.46895(11) 0.1963(2) 0.0574(7) Uani 1 d . .
H11A H 0.3549(3) 0.50457(11) 0.1753(2) 0.069 Uiso 1 calc R .
H11B H 0.2225(3) 0.47272(11) 0.2115(2) 0.069 Uiso 1 calc R .
C12 C 0.4280(3) 0.44926(11) 0.3185(3) 0.0511(7) Uani 1 d . .
C13 C 0.3894(3) 0.40818(11) 0.3931(3) 0.0591(8) Uani 1 d . .
H13A H 0.2958(3) 0.39165(11) 0.3661(3) 0.071 Uiso 1 calc R .
C14 C 0.4858(3) 0.39092(11) 0.5068(3) 0.0597(8) Uani 1 d . .
H14A H 0.4571(3) 0.36316(11) 0.5551(3) 0.072 Uiso 1 calc R .
C15 C 0.6245(3) 0.41523(12) 0.5478(3) 0.0558(7) Uani 1 d . .
C16 C 0.6671(3) 0.45545(12) 0.4738(3) 0.0581(7) Uani 1 d . .
H16A H 0.7613(3) 0.47161(12) 0.5002(3) 0.070 Uiso 1 calc R .
C17 C 0.5705(3) 0.47141(11) 0.3616(3) 0.0568(7) Uani 1 d . .
H17A H 0.6014(3) 0.49820(11) 0.3120(3) 0.068 Uiso 1 calc R .
C18 C 0.6786(4) 0.3706(2) 0.7525(3) 0.0963(12) Uani 1 d . .
H18A H 0.7554(11) 0.3698(8) 0.8315(8) 0.116 Uiso 1 calc R .
H18B H 0.6594(24) 0.3344(3) 0.7196(9) 0.116 Uiso 1 calc R .
H18C H 0.5880(14) 0.3856(5) 0.7687(16) 0.116 Uiso 1 calc R .
C19 C 0.5328(3) 0.37144(10) 0.1028(2) 0.0430(6) Uani 1 d . .
C20 C 0.7866(3) 0.33240(11) 0.1626(3) 0.0549(7) Uani 1 d . .
C21 C 0.9364(3) 0.35843(14) 0.1619(4) 0.0974(13) Uani 1 d . .
H21A H 0.9363(9) 0.3699(8) 0.0757(5) 0.117 Uiso 1 calc R .
H21B H 1.0158(4) 0.3326(3) 0.1910(20) 0.117 Uiso 1 calc R .
H21C H 0.9521(11) 0.3893(5) 0.2187(16) 0.117 Uiso 1 calc R .
C22 C 0.7772(4) 0.31891(13) 0.2986(3) 0.0805(10) Uani 1 d . .
H22A H 0.6829(10) 0.3014(7) 0.2966(3) 0.097 Uiso 1 calc R .
H22B H 0.7842(21) 0.3517(2) 0.3485(6) 0.097 Uiso 1 calc R .
H22C H 0.8584(13) 0.2951(6) 0.3374(7) 0.097 Uiso 1 calc R .
C23 C 0.7572(4) 0.28340(13) 0.0753(3) 0.0881(11) Uani 1 d . .
H23A H 0.7585(23) 0.2939(2) -0.0113(5) 0.106 Uiso 1 calc R .
H23B H 0.6606(11) 0.2684(5) 0.0761(15) 0.106 Uiso 1 calc R .
H23C H 0.8339(14) 0.2567(4) 0.1056(12) 0.106 Uiso 1 calc R .
