#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/91/4109103.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_4109103
loop_
_publ_author_name
'Paul V. Santacroce'
'Jeffery T. Davis'
'Mark E. Light'
'Philip A. Gale'
'José Carlos Iglesias-Sánchez'
'Pilar Prados'
'Roberto Quesada'
_publ_section_title
;
 Conformational Control of Transmembrane Cl-Transport
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1886
_journal_page_last               1887
_journal_paper_doi               10.1021/ja068067v
_journal_volume                  129
_journal_year                    2007
_chemical_compound_source        'Roberto Quesada'
_chemical_formula_sum            'C18 H28 N2 O4'
_chemical_formula_weight         336.42
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.437(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6110(11)
_cell_length_b                   8.4257(4)
_cell_length_c                   15.6598(12)
_cell_measurement_reflns_used    7526
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1776.5(2)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22428
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_correction_T_min  0.9725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       Rod
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0673P)²+0.1681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                2224
_reflns_number_total             4053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068067vsi20061117_100153_1.cif
_cod_data_source_block           2006sot1099
_cod_database_code               4109103
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.3890(2) 0.6400(3) 0.01202(19) 0.0342(7) Uani 1 1 d .
H1A H 0.4306 0.5766 0.0557 0.051 Uiso 1 1 calc R
H1B H 0.4234 0.7389 0.0021 0.051 Uiso 1 1 calc R
H1C H 0.3759 0.5798 -0.0420 0.051 Uiso 1 1 calc R
C2 C 0.2910(2) 0.6784(3) 0.04356(17) 0.0255(6) Uani 1 1 d .
H2A H 0.3049 0.7363 0.0990 0.031 Uiso 1 1 calc R
H2B H 0.2516 0.7492 0.0012 0.031 Uiso 1 1 calc R
C3 C 0.2299(2) 0.5312(3) 0.05622(18) 0.0256(6) Uani 1 1 d .
H3A H 0.2167 0.4720 0.0011 0.031 Uiso 1 1 calc R
H3B H 0.2685 0.4613 0.0996 0.031 Uiso 1 1 calc R
C4 C 0.1324(2) 0.5734(3) 0.08585(17) 0.0240(6) Uani 1 1 d .
H4A H 0.1457 0.6389 0.1388 0.029 Uiso 1 1 calc R
H4B H 0.0923 0.6379 0.0407 0.029 Uiso 1 1 calc R
C5 C -0.0136(2) 0.4497(3) 0.12919(16) 0.0225(6) Uani 1 1 d .
C6 C -0.0704(2) 0.3022(3) 0.14656(15) 0.0215(6) Uani 1 1 d .
C7 C -0.0399(2) 0.1443(3) 0.13875(16) 0.0226(6) Uani 1 1 d .
C8 C -0.1002(2) 0.0184(3) 0.15640(16) 0.0217(6) Uani 1 1 d .
H8 H -0.0788 -0.0879 0.1506 0.026 Uiso 1 1 calc R
C9 C -0.1911(2) 0.0481(2) 0.18232(16) 0.0213(6) Uani 1 1 d .
C10 C -0.22575(19) 0.2051(3) 0.19022(16) 0.0214(6) Uani 1 1 d .
C11 C -0.1629(2) 0.3259(3) 0.17167(16) 0.0225(6) Uani 1 1 d .
H11 H -0.1847 0.4322 0.1765 0.027 Uiso 1 1 calc R
C12 C -0.3233(2) 0.2554(3) 0.21508(16) 0.0221(6) Uani 1 1 d .
C13 C -0.48979(19) 0.1805(3) 0.24392(17) 0.0243(6) Uani 1 1 d .
H13A H -0.4860 0.2712 0.2845 0.029 Uiso 1 1 calc R
H13B H -0.5165 0.0883 0.2722 0.029 Uiso 1 1 calc R
C14 C -0.5603(2) 0.2220(3) 0.16253(17) 0.0265(7) Uani 1 1 d .
H14A H -0.5326 0.3128 0.1338 0.032 Uiso 1 1 calc R
H14B H -0.6246 0.2563 0.1789 0.032 Uiso 1 1 calc R
C15 C -0.5789(2) 0.0854(3) 0.09871(18) 0.0303(7) Uani 1 1 d .
H15A H -0.5147 0.0514 0.0822 0.036 Uiso 1 1 calc R
H15B H -0.6065 -0.0054 0.1276 0.036 Uiso 1 1 calc R
C16 C -0.6494(2) 0.1264(3) 0.01776(18) 0.0367(8) Uani 1 1 d .
H16A H -0.7140 0.1567 0.0333 0.055 Uiso 1 1 calc R
H16B H -0.6575 0.0340 -0.0206 0.055 Uiso 1 1 calc R
H16C H -0.6222 0.2151 -0.0118 0.055 Uiso 1 1 calc R
C17 C 0.0847(2) -0.0405(3) 0.10608(19) 0.0319(7) Uani 1 1 d .
H17A H 0.0870 -0.0937 0.1620 0.048 Uiso 1 1 calc R
H17B H 0.1513 -0.0394 0.0894 0.048 Uiso 1 1 calc R
H17C H 0.0391 -0.0975 0.0623 0.048 Uiso 1 1 calc R
C18 C -0.2205(2) -0.2336(2) 0.19265(18) 0.0281(7) Uani 1 1 d .
H18A H -0.2082 -0.2516 0.1333 0.042 Uiso 1 1 calc R
H18B H -0.2724 -0.3064 0.2060 0.042 Uiso 1 1 calc R
H18C H -0.1593 -0.2527 0.2327 0.042 Uiso 1 1 calc R
N1 N 0.07561(16) 0.4344(2) 0.10357(14) 0.0250(5) Uani 1 1 d .
H1 H 0.1001 0.3391 0.0974 0.030 Uiso 1 1 calc R
N2 N -0.39028(16) 0.1429(2) 0.22635(14) 0.0240(5) Uani 1 1 d .
H2 H -0.3733 0.0426 0.2230 0.029 Uiso 1 1 calc R
O1 O -0.04884(14) 0.58192(18) 0.13902(12) 0.0337(5) Uani 1 1 d .
O2 O -0.34059(14) 0.39732(18) 0.22465(12) 0.0311(5) Uani 1 1 d .
O3 O 0.05059(14) 0.11954(17) 0.11276(12) 0.0279(5) Uani 1 1 d .
O4 O -0.25253(14) -0.07184(17) 0.20154(11) 0.0270(5) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C3 C2 C1 113.0(2)
C4 C3 C2 111.70(19)
N1 C4 C3 112.63(18)
O1 C5 N1 120.7(2)
O1 C5 C6 120.2(2)
N1 C5 C6 119.0(2)
C11 C6 C7 116.9(2)
C11 C6 C5 116.3(2)
C7 C6 C5 126.8(2)
O3 C7 C8 121.7(2)
O3 C7 C6 117.5(2)
C8 C7 C6 120.9(2)
C9 C8 C7 120.0(2)
O4 C9 C8 122.11(19)
O4 C9 C10 116.5(2)
C8 C9 C10 121.4(2)
C11 C10 C9 116.3(2)
C11 C10 C12 116.4(2)
C9 C10 C12 127.3(2)
C10 C11 C6 124.6(2)
O2 C12 N2 121.5(2)
O2 C12 C10 119.9(2)
N2 C12 C10 118.6(2)
N2 C13 C14 112.5(2)
C13 C14 C15 113.6(2)
C16 C15 C14 113.7(2)
C5 N1 C4 120.68(19)
C12 N2 C13 122.61(19)
C7 O3 C17 118.70(18)
C9 O4 C18 118.14(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.523(4)
C2 C3 1.522(3)
C3 C4 1.512(3)
C4 N1 1.452(3)
C5 O1 1.231(3)
C5 N1 1.340(3)
C5 C6 1.509(3)
C6 C11 1.387(3)
C6 C7 1.404(3)
C7 O3 1.369(3)
C7 C8 1.394(3)
C8 C9 1.379(3)
C9 O4 1.374(3)
C9 C10 1.416(3)
C10 C11 1.387(3)
C10 C12 1.499(3)
C12 O2 1.232(3)
C12 N2 1.344(3)
C13 N2 1.456(3)
C13 C14 1.520(4)
C14 C15 1.521(3)
C15 C16 1.513(4)
C17 O3 1.435(3)
C18 O4 1.444(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660354
