#------------------------------------------------------------------------------
#$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $
#$Revision: 481 $
#$URL: svn://www.crystallography.net/cod/cif/2/2002104.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_2002104
_journal_name_full 'Acta Crystallographica Section C'
_journal_year 1993
_journal_volume 49
_journal_page_first 171
_journal_page_last 173
_publ_section_title
;
Structure of Kopsine: Methyl 3-Hydroxy-22-oxokopsan-1-carboxylate
;
loop_
_publ_author_name
'Watt, William'
'Ghosh, Ratna'
'Seal, Tapan'
'Mukherjee, Biswapati'
_chemical_name_systematic
;
'Methyl 3-Hydroxy-22-oxokopsan-1-carboxylate'
;
_chemical_formula_sum 'C22 H24 N2 O4'
_chemical_formula_weight 380.43
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P 21 21 21'
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
_cell_length_a 10.193(3)
_cell_length_b 11.9660(10)
_cell_length_c 14.802(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1805.4(7)
_cell_formula_units_z 4
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 60
_cell_measurement_theta_max 68
_cell_measurement_temperature 158
_exptl_crystal_description 'chunky block'
_exptl_crystal_colour clear
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.48
_exptl_crystal_density_diffrn 1.40
_exptl_crystal_density_meas ?
_exptl_crystal_F_000 808
_exptl_absorpt_coefficient_mu 0.699
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_diffrn_ambient_temperature 158
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'Siemens P2~1~'
_diffrn_measurement_method \q/2\q
_diffrn_reflns_number 1775
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_sigmaI/netI ?
_diffrn_reflns_theta_min 1
_diffrn_reflns_theta_max 68
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_reduction_process ?
_diffrn_standards_number 10
_diffrn_standards_interval_count 80
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 0 1
1 1 -6
2 1 4
2 2 0
0 3 1
1 3 5
-2 4 2
1 4 0
0 5 -1
1 5 1
_reflns_number_total 1775
_reflns_number_observed 1689
_reflns_observed_criterion refl_observed_if_I_>_3.0sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.047
_refine_ls_R_factor_obs 0.045
_refine_ls_wR_factor_all 0.123
_refine_ls_wR_factor_obs 0.122
_refine_ls_goodness_of_fit_all 4.80
_refine_ls_goodness_of_fit_obs ?
_refine_ls_number_reflns 1772
_refine_ls_number_parameters 349
_refine_ls_number_restraints ?
_refine_ls_number_constraints ?
_refine_ls_hydrogen_treatment noref
_refine_ls_weighting_scheme 'calc w = 1/[\s^2^(F^2^)]'
_refine_ls_shift/esd_max 0.020
_refine_ls_shift/esd_mean 0.017
_refine_diff_density_max 0.314
_refine_diff_density_min -0.32
_refine_ls_extinction_method ?
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details
;
The absolute configuration was established by nmr
(Guggisberg, Gorman, Bycroft \& Schmid, 1969)
;
_refine_ls_abs_structure_Flack ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.017 0.009 'Cromer \& Liberman, 1970'
H 0 0 'International Tables Vol.IV Table 2.3.1'
N 0.029 0.018 'Cromer \& Liberman, 1970'
O 0.047 0.032 'Cromer \& Liberman, 1970'
_computing_data_reduction
;
performed using the program of Duchamp (1977)
;
_computing_structure_solution
;
MULTAN (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1980)
;
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
C(1) -0.7144(4) -0.2750(3) -0.7167(2) Bani ? ?
N(2) -0.8026(3) -0.2595(2) -0.7970(2) Bani ? ?
C(1') -0.7707(4) -0.1927(3) -0.8683(2) Bani ? ?
O(1') -0.6634(3) -0.1515(2) -0.8814(2) Bani ? ?
O(2') -0.8718(3) -0.1789(2) -0.9256(2) Bani ? ?
C(3') -0.8381(4) -0.1217(4) -1.0093(2) Bani ? ?
C(3) -0.5729(4) -0.3196(3) -0.7328(2) Bani ? ?
O(3) -0.4842(3) -0.2575(2) -0.7851(2) Bani ? ?
C(4) -0.5120(4) -0.3311(3) -0.6351(2) Bani ? ?
C(5) -0.6129(4) -0.3135(3) -0.5580(2) Bani ? ?
C(6) -0.5527(4) -0.3416(3) -0.4655(2) Bani ? ?
C(7) -0.5334(4) -0.4674(3) -0.4523(2) Bani ? ?
C(8) -0.6643(4) -0.5289(3) -0.4669(2) Bani ? ?
N(9) -0.7282(3) -0.5037(2) -0.5536(2) Bani ? ?
C(10) -0.6677(4) -0.5581(3) -0.6325(2) Bani ? ?
C(11) -0.7111(4) -0.4848(3) -0.7132(2) Bani ? ?
C(12) -0.7783(4) -0.3786(3) -0.6710(2) Bani ? ?
C(13) -0.9195(4) -0.3693(3) -0.6966(2) Bani ? ?
C(14) -1.0250(4) -0.4225(3) -0.6591(2) Bani ? ?
C(15) -1.1479(4) -0.4039(3) -0.6970(2) Bani ? ?
C(16) -1.1618(4) -0.3321(3) -0.7698(2) Bani ? ?
C(17) -1.0543(4) -0.2794(3) -0.8094(2) Bani ? ?
C(18) -0.9306(4) -0.2998(3) -0.7717(2) Bani ? ?
C(19) -0.7373(4) -0.3841(3) -0.5716(2) Bani ? ?
C(20) -0.6525(4) -0.1907(3) -0.5646(2) Bani ? ?
C(21) -0.7166(4) -0.1688(3) -0.6585(2) Bani ? ?
C(22) -0.5970(4) -0.4377(3) -0.7671(2) Bani ? ?
O(22) -0.5373(3) -0.4843(2) -0.8266(2) Bani ? ?
H(O3) -0.519 -0.251 -0.848 Biso ? ?
H(4A) -0.474 -0.407 -0.628 Biso ? ?
H(4B) -0.440 -0.274 -0.627 Biso ? ?
H(6A) -0.465 -0.303 -0.460 Biso ? ?
H(6B) -0.612 -0.312 -0.417 Biso ? ?
H(7A) -0.468 -0.495 -0.496 Biso ? ?
H(7B) -0.502 -0.481 -0.389 Biso ? ?
H(8A) -0.646 -0.611 -0.464 Biso ? ?
H(8B) -0.725 -0.507 -0.416 Biso ? ?
H(10A) -0.570 -0.558 -0.626 Biso ? ?
H(10B) -0.700 -0.636 -0.639 Biso ? ?
H(11) -0.773 -0.525 -0.753 Biso ? ?
H(14) -1.014 -0.472 -0.605 Biso ? ?
H(15) -1.227 -0.442 -0.671 Biso ? ?
H(16) -1.251 -0.317 -0.794 Biso ? ?
H(17) -1.064 -0.228 -0.862 Biso ? ?
H(19) -0.808 -0.352 -0.533 Biso ? ?
H(20A) -0.717 -0.173 -0.515 Biso ? ?
H(20B) -0.573 -0.141 -0.557 Biso ? ?
H(21A) -0.666 -0.108 -0.690 Biso ? ?
H(21B) -0.809 -0.145 -0.649 Biso ? ?
H(3'A) -0.918 -0.114 -1.047 Biso ? ?
H(3'B) -0.803 -0.045 -0.994 Biso ? ?
H(3'C) -0.769 -0.165 -1.042 Biso ? ?