#------------------------------------------------------------------------------
#$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/04/2010496.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010496
loop_
_publ_author_name
'Nurit, J.'
'Rambaud, J.'
'Pauvert, B.'
'Doumbia, O.'
'T\'erol, A.'
'Chevallet, P.'
'Declercq, J.-P.'
_publ_section_title
;
 Polymorph (II) of Methyl
 3-(4-Ethoxy-\a-hydroxyiminobenzyl)-1,2,2-trimethyl-cyclopentanecarboxylate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              322
_journal_page_last               324
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C19 H27 N O4'
_chemical_formula_weight         333.428
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 125.620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.179(2)
_cell_length_b                   11.2030(10)
_cell_length_c                   17.286(2)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     3806.3(8)
_diffrn_measurement_device       'Huber four circle'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3432
_diffrn_reflns_theta_max         67.5
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.16
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none?
_refine_ls_goodness_of_fit_obs   1.53
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2850
_refine_ls_R_factor_obs          0.058
_refine_ls_shift/esd_max         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'w = 1/[\s^2^(F) + 0.005315F^2^]'
_refine_ls_wR_factor_obs         0.088
_reflns_number_observed          2850
_reflns_number_total             3432
_reflns_observed_criterion       I>=2.5\s
_[local]_cod_data_source_file    pa1101.cif
_[local]_cod_data_source_block   pa1101_structure_1_of_1
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
_[local]_cod_chemical_formula_sum_orig 'C19 H27 N1 O4'
_cod_original_cell_volume        3806.0(10)
_cod_database_code               2010496
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,-y,1/2+z
-x,-y,-z
-x,y,1/2-z
1/2+x,1/2+y,z
1/2+x,1/2-y,1/2+z
1/2-x,1/2-y,-z
1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C(1) -.74840(10) .4269(2) -.34020(10)
C(11) -.77060(10) .5256(2) -.4123(2)
C(12) -.80010(10) .3248(3) -.3881(2)
C(2) -.67300(10) .3861(2) -.29620(10)
C(21) -.6679(2) .2891(4) -.3538(2)
C(22) -.6304(2) .4922(4) -.2858(3)
C(3) -.65010(10) .3388(2) -.1977(2)
C(31) -.57420(10) .3175(2) -.1278(2)
C(32) -.54540(10) .2011(2) -.12930(10)
C(33) -.48780(10) .1941(2) -.1294(2)
C(34) -.46220(10) .0851(2) -.1304(2)
C(35) -.49150(10) -.0197(2) -.12880(10)
C(36) -.54870(10) -.0145(2) -.12830(10)
C(37) -.57500(10) .0953(2) -.12860(10)
C(38) -.48720(10) -.2329(2) -.1218(2)
C(39) -.4400(2) -.3292(3) -.1101(2)
C(4) -.68230(10) .4236(3) -.16550(10)
C(41) -.7948(2) .5745(4) -.5622(2)
C(5) -.74600(10) .4711(3) -.2542(2)
N -.53920(10) .4027(2) -.07070(10)
O(1) -.46070(10) -.12230(10) -.12690(10)
O(2) -.46870(10) .37770(10) -.00670(10)
O(3) -.78080(10) .6272(2) -.4026(2)
O(4) -.77770(10) .4869(2) -.49090(10)
H34 -.41850(10) .0814(2) -.1325(2)
H33 -.46330(10) .2751(2) -.1289(2)
H37 -.61960(10) .0988(2) -.1285(2)
H36 -.57240(10) -.0957(2) -.1276(2)
H3 -.6734(11) .262(2) -.2071(15)
H4 -.64790(10) .4960(3) -.1247(2)
H4' -.69440(10) .3765(3) -.1227(2)
H5 -.79000(10) .4388(3) -.2589(2)
H5' -.74560(10) .5675(3) -.2527(2)
H38 -.49010(10) -.2327(2) -.0618(2)
H38' -.53730(10) -.2471(2) -.1865(2)
H39 -.4589(2) -.4149(3) -.1062(2)
H39' -.3899(2) -.3140(3) -.0455(2)
H39" -.4372(2) -.3283(3) -.1703(2)
H21 -.6984(2) .2133(4) -.3618(2)
H21' -.6155(2) .2618(4) -.3171(2)
H21" -.6861(2) .3236(4) -.4232(2)
H22 -.63390(10) .5611(3) -.2452(3)
H22' -.64860(10) .5264(3) -.3553(3)
H22" -.57800(10) .4646(3) -.2492(3)
H12 -.78500(10) .2533(3) -.3377(2)
H12' -.80160(10) .2928(3) -.4481(2)
H12" -.84990(10) .3568(3) -.4123(2)
H41 -.7988(2) .5319(4) -.6218(2)
H41' -.7556(2) .6420(4) -.5322(2)
H41" -.8429(2) .6154(4) -.5868(2)
H -.438(2) .465(4) .056(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C(34) C(35) . . 1.380(3) yes
C(36) C(35) . . 1.388(3) yes
O(1) C(35) . . 1.359(3) yes
C(33) C(34) . . 1.374(3) yes
C(32) C(33) . . 1.396(3) yes
C(37) C(32) . . 1.388(3) yes
C(31) C(32) . . 1.484(3) yes
C(36) C(37) . . 1.384(3) yes
C(3) C(31) . . 1.518(2) yes
N C(31) . . 1.274(2) yes
C(4) C(3) . . 1.522(3) yes
C(2) C(3) . . 1.547(3) yes
C(5) C(4) . . 1.502(3) yes
C(1) C(5) . . 1.537(3) yes
C(2) C(1) . . 1.580(2) yes
C(12) C(1) . . 1.533(3) yes
C(11) C(1) . . 1.512(3) yes
C(21) C(2) . . 1.525(3) yes
C(22) C(2) . . 1.513(4) yes
C(39) C(38) . . 1.496(3) yes
O(1) C(38) . . 1.421(3) yes
O(3) C(11) . . 1.197(3) yes
O(4) C(11) . . 1.338(3) yes
O(4) C(41) . . 1.435(3) yes
O(2) N . . 1.417(2) yes
H34 C(34) . . 1.080 no
H33 C(33) . . 1.080 no
H37 C(37) . . 1.080 no
H36 C(36) . . 1.080 no
H3 C(3) . . 0.993 no
H4 C(4) . . 1.080 no
H4' C(4) . . 1.080 no
H5 C(5) . . 1.080 no
H5' C(5) . . 1.080 no
H38 C(38) . . 1.080 no
H38' C(38) . . 1.080 no
H39 C(39) . . 1.080 no
H39' C(39) . . 1.080 no
H39" C(39) . . 1.080 no
H21 C(21) . . 1.080 no
H21' C(21) . . 1.080 no
H21" C(21) . . 1.080 no
H22 C(22) . . 1.080 no
H22' C(22) . . 1.080 no
H22" C(22) . . 1.080 no
H12 C(12) . . 1.080 no
H12' C(12) . . 1.080 no
H12" C(12) . . 1.080 no
H41 C(41) . . 1.080 no
H41' C(41) . . 1.080 no
H41" C(41) . . 1.080 no
H O(2) . . 1.317 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C(36) C(35) C(34) 119.3(2) yes
O(1) C(35) C(34) 116.1(2) yes
O(1) C(35) C(36) 124.7(2) yes
C(33) C(34) C(35) 121.1(2) yes
C(32) C(33) C(34) 120.5(2) yes
C(37) C(32) C(33) 118.1(2) yes
C(31) C(32) C(33) 121.8(2) yes
C(31) C(32) C(37) 120.1(2) yes
C(36) C(37) C(32) 121.4(2) yes
C(37) C(36) C(35) 119.7(2) yes
C(3) C(31) C(32) 119.1(2) yes
N C(31) C(32) 124.3(2) yes
N C(31) C(3) 116.6(2) yes
C(4) C(3) C(31) 116.5(2) yes
C(2) C(3) C(31) 114.9(2) yes
C(2) C(3) C(4) 104.9(2) yes
C(5) C(4) C(3) 106.7(2) yes
C(1) C(5) C(4) 108.1(2) yes
C(2) C(1) C(5) 104.2(2) yes
C(12) C(1) C(5) 108.8(2) yes
C(12) C(1) C(2) 113.2(2) yes
C(11) C(1) C(5) 110.9(2) yes
C(11) C(1) C(2) 111.4(2) yes
C(11) C(1) C(12) 108.3(2) yes
C(1) C(2) C(3) 101.60(10) yes
C(21) C(2) C(3) 111.2(2) yes
C(21) C(2) C(1) 113.6(2) yes
C(22) C(2) C(3) 110.9(2) yes
C(22) C(2) C(1) 110.2(2) yes
C(22) C(2) C(21) 109.2(3) yes
O(1) C(38) C(39) 107.5(2) yes
O(3) C(11) C(1) 125.6(2) yes
O(4) C(11) C(1) 111.9(2) yes
O(4) C(11) O(3) 122.5(3) yes
O(2) N C(31) 114.2(2) yes
C(38) O(1) C(35) 118.5(2) yes
C(41) O(4) C(11) 116.9(2) yes
H34 C(34) C(35) 119.50(10) no
C(33) C(34) H34 119.40(10) no
H33 C(33) C(34) 119.90(10) no
C(32) C(33) H33 119.70(10) no
H37 C(37) C(32) 119.20(10) no
C(36) C(37) H37 119.30(10) no
H36 C(36) C(35) 120.20(10) no
H36 C(36) C(37) 120.10(10) no
H3 C(3) C(31) 107.5(13) no
C(4) C(3) H3 104.0(13) no
C(2) C(3) H3 108.3(13) no
H4 C(4) C(3) 110.10(10) no
H4' C(4) C(3) 110.20(10) no
C(5) C(4) H4 110.10(10) no
C(5) C(4) H4' 110.2(2) no
H5 C(5) C(4) 109.8(2) no
H5' C(5) C(4) 109.9(2) no
C(1) C(5) H5 109.8(2) no
C(1) C(5) H5' 109.8(2) no
C(39) C(38) H38 110.0(2) no
C(39) C38) H38' 110.0(2) no
O(1) C(38) H38 110.00(10) no
O(1) C(38) H38' 109.90(10) no
H39 C(39) C(38) 109.3(2) no
H39' C(39) C(38) 109.5(2) no
H39' C(39) H39 109.5(2) no
H21 C(21) C(2) 109.6(2) no
H21' C(21) C(2) 109.30(10) no
H21" C(21) C(2) 109.5(2) no
H22 C(22) C(2) 109.5(2) no
H22' C(22) C(2) 109.7(2) no
H22" C(22) C(2) 109.30(10) no
H12 C(12) C(1) 109.40(10) no
H12' C(12) C(1) 109.30(10) no
_journal_paper_doi 10.1107/S0108270194006013