#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:19:08 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180387 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/56/7205637.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_7205637
loop_
_publ_author_name
'Wahl, Helene'
'Haynes, Delia A.'
'le Roex, Tanya'
_publ_section_title
;
 Solvate formation in lutidinium pamoate salts: a systematic study
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              2227
_journal_paper_doi               10.1039/c0ce00528b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C7 H10 N 1+ , C23 H15 O6 1- , C4 H8 O'
_chemical_formula_sum            'C34 H33 N O7'
_chemical_formula_weight         567.61
_chemical_name_common            '2,5 lutidinium pamoate THF solvate'
_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                 112.830(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.820(8)
_cell_length_b                   12.922(8)
_cell_length_c                   17.143(10)
_cell_measurement_reflns_used    2536
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.104
_cell_measurement_theta_min      2.451
_cell_volume                     2822(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15747
_diffrn_reflns_theta_full        26.24
_diffrn_reflns_theta_max         26.24
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_correction_T_min  0.9854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.426
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.426
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.1191
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3655
_refine_ls_wR_factor_ref         0.4166
_reflns_number_gt                3154
_reflns_number_total             5679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00528b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7205637
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N11 N 0.7271(5) 0.6409(4) -0.0672(4) 0.0965(19) Uani 1 1 d . . .
H11 H 0.7257 0.6693 -0.0210 0.116 Uiso 1 1 calc R . .
C12 C 0.6407(6) 0.5779(5) -0.1188(5) 0.096(2) Uani 1 1 d . . .
C13 C 0.6530(5) 0.5388(4) -0.1885(4) 0.0730(15) Uani 1 1 d . . .
H13 H 0.5999 0.4953 -0.2261 0.088 Uiso 1 1 calc R . .
C14 C 0.7355(6) 0.5595(6) -0.2045(6) 0.113(3) Uani 1 1 d . . .
H14 H 0.7376 0.5302 -0.2547 0.135 Uiso 1 1 calc R . .
C15 C 0.8176(5) 0.6177(6) -0.1582(4) 0.0900(19) Uani 1 1 d . . .
C16 C 0.8076(5) 0.6571(5) -0.0870(4) 0.0850(18) Uani 1 1 d . . .
H16 H 0.8631 0.6988 -0.0501 0.102 Uiso 1 1 calc R . .
C17 C 0.5568(7) 0.5614(7) -0.0911(6) 0.136(3) Uani 1 1 d . . .
H17A H 0.5854 0.5374 -0.0323 0.205 Uiso 1 1 calc R . .
H17B H 0.5088 0.5091 -0.1271 0.205 Uiso 1 1 calc R . .
H17C H 0.5187 0.6264 -0.0950 0.205 Uiso 1 1 calc R . .
C18 C 0.9133(8) 0.6336(11) -0.1749(8) 0.208(7) Uani 1 1 d . . .
H18A H 0.9654 0.5809 -0.1449 0.311 Uiso 1 1 calc R . .
H18B H 0.9421 0.7025 -0.1551 0.311 Uiso 1 1 calc R . .
H18C H 0.8961 0.6281 -0.2358 0.311 Uiso 1 1 calc R . .
O31 O 0.8044(7) 0.5035(8) -0.3757(6) 0.145(3) Uiso 0.68 1 d P A 1
C31 C 0.8112(9) 0.4111(10) -0.4057(7) 0.110(3) Uiso 0.68 1 d P A 1
C32 C 0.9026(10) 0.3857(11) -0.4105(8) 0.177(4) Uiso 1 1 d . . .
C33 C 0.8890(9) 0.5597(9) -0.3886(8) 0.109(3) Uiso 0.68 1 d P A 1
C34 C 0.9765(12) 0.4903(12) -0.3607(10) 0.144(5) Uiso 0.68 1 d P A 1
C35 C 1.031(2) 0.508(2) -0.402(2) 0.133(9) Uiso 0.33 1 d P A -1
C36 C 0.867(2) 0.472(2) -0.4764(19) 0.133(9) Uiso 0.33 1 d P A -1
C37 C 1.007(3) 0.411(3) -0.421(2) 0.149(10) Uiso 0.33 1 d P A -1
O41 O 0.924(3) 0.560(3) -0.440(2) 0.236(13) Uiso 0.33 1 d P A -1
O211 O 0.5608(2) 0.8177(2) 0.0972(2) 0.0622(10) Uani 1 1 d . . .
H211 H 0.6111 0.8127 0.0815 0.075 Uiso 1 1 calc R . .
C211 C 0.5775(3) 0.7537(3) 0.1641(3) 0.0475(11) Uani 1 1 d . . .
C212 C 0.6729(3) 0.6931(3) 0.1972(3) 0.0493(11) Uani 1 1 d . . .
C213 C 0.6918(3) 0.6339(3) 0.2665(3) 0.0476(11) Uani 1 1 d . . .
H213 H 0.7540 0.5933 0.2876 0.057 Uiso 1 1 calc R . .
C214 C 0.6216(3) 0.6306(3) 0.3086(3) 0.0427(10) Uani 1 1 d . . .
C215 C 0.6445(4) 0.5737(3) 0.3839(3) 0.0515(11) Uani 1 1 d . . .
H215 H 0.7078 0.5349 0.4062 0.062 Uiso 1 1 calc R . .
C216 C 0.5789(4) 0.5730(3) 0.4249(3) 0.0556(12) Uani 1 1 d . . .
H216 H 0.5958 0.5341 0.4755 0.067 Uiso 1 1 calc R . .
C217 C 0.4848(4) 0.6304(3) 0.3923(3) 0.0506(11) Uani 1 1 d . . .
H217 H 0.4388 0.6303 0.4215 0.061 Uiso 1 1 calc R . .
C218 C 0.4590(3) 0.6858(3) 0.3197(3) 0.0444(10) Uani 1 1 d . . .
H218 H 0.3948 0.7232 0.2987 0.053 Uiso 1 1 calc R . .
C219 C 0.5265(3) 0.6892(3) 0.2741(2) 0.0396(9) Uani 1 1 d . . .
C220 C 0.5043(3) 0.7490(3) 0.2009(3) 0.0402(9) Uani 1 1 d . . .
C221 C 0.7494(4) 0.6961(4) 0.1540(4) 0.0676(15) Uani 1 1 d . . .
O221 O 0.7230(3) 0.7380(4) 0.0834(3) 0.1083(18) Uani 1 1 d . . .
O222 O 0.8381(2) 0.6538(3) 0.1944(2) 0.0664(10) Uani 1 1 d . . .
C222 C 0.4034(3) 0.8136(3) 0.1629(3) 0.0419(10) Uani 1 1 d . . .
H22A H 0.3989 0.8592 0.2078 0.050 Uiso 1 1 calc R . .
H22B H 0.4092 0.8586 0.1182 0.050 Uiso 1 1 calc R . .
C223 C 0.3022(3) 0.7527(3) 0.1253(2) 0.0372(9) Uani 1 1 d . . .
C224 C 0.2275(3) 0.7580(3) 0.1604(3) 0.0384(9) Uani 1 1 d . . .
O224 O 0.2447(2) 0.8226(2) 0.22701(18) 0.0459(8) Uani 1 1 d . . .
H224 H 0.190(3) 0.811(3) 0.238(3) 0.051(13) Uiso 1 1 d . . .
C225 C 0.1333(3) 0.6983(3) 0.1268(3) 0.0431(10) Uani 1 1 d . . .
C226 C 0.1165(3) 0.6340(3) 0.0595(3) 0.0416(10) Uani 1 1 d . . .
H226 H 0.0557 0.5915 0.0398 0.050 Uiso 1 1 calc R . .
C227 C 0.1869(3) 0.6296(3) 0.0191(3) 0.0436(10) Uani 1 1 d . . .
C228 C 0.1661(4) 0.5679(3) -0.0540(3) 0.0562(12) Uani 1 1 d . . .
H228 H 0.1067 0.5234 -0.0728 0.067 Uiso 1 1 calc R . .
C229 C 0.2291(5) 0.5713(4) -0.0974(3) 0.0669(14) Uani 1 1 d . . .
H229 H 0.2132 0.5305 -0.1469 0.080 Uiso 1 1 calc R . .
C230 C 0.3177(4) 0.6348(4) -0.0695(3) 0.0608(13) Uani 1 1 d . . .
H230 H 0.3597 0.6391 -0.1020 0.073 Uiso 1 1 calc R . .
C231 C 0.3453(3) 0.6912(3) 0.0040(3) 0.0500(11) Uani 1 1 d . . .
H231 H 0.4083 0.7306 0.0235 0.060 Uiso 1 1 calc R . .
C232 C 0.2800(3) 0.6911(3) 0.0512(3) 0.0408(9) Uani 1 1 d . . .
C233 C 0.0546(3) 0.7056(3) 0.1664(3) 0.0490(11) Uani 1 1 d . . .
O233 O 0.0692(2) 0.7606(2) 0.2284(2) 0.0577(9) Uani 1 1 d . . .
O234 O -0.0300(2) 0.6522(3) 0.1280(3) 0.0688(11) Uani 1 1 d . . .
H234 H -0.0707 0.6591 0.1536 0.083 Uiso 1 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 N11 C12 121.5(7) . . ?
C13 C12 C17 128.8(8) . . ?
C13 C12 N11 113.2(7) . . ?
C17 C12 N11 118.0(8) . . ?
C14 C13 C12 121.7(7) . . ?
C13 C14 C15 127.0(9) . . ?
C14 C15 C16 112.4(7) . . ?
C14 C15 C18 125.6(9) . . ?
C16 C15 C18 121.8(9) . . ?
N11 C16 C15 124.2(7) . . ?
C31 O31 C33 102.0(10) . . ?
O31 C31 C32 117.3(12) . . ?
O31 C31 C36 88.7(12) . . ?
C32 C31 C36 54.8(10) . . ?
C31 C32 C36 79.7(14) . . ?
C31 C32 C37 153.6(18) . . ?
C36 C32 C37 79.2(18) . . ?
C31 C32 C34 99.8(11) . . ?
C36 C32 C34 75.5(14) . . ?
C37 C32 C34 59.6(14) . . ?
O41 C33 C34 73.3(19) . . ?
O41 C33 O31 135(2) . . ?
C34 C33 O31 105.1(11) . . ?
O41 C33 C36 50.0(19) . . ?
C34 C33 C36 74.8(12) . . ?
O31 C33 C36 85.8(12) . . ?
C35 C34 C33 109(2) . . ?
C35 C34 O41 64.9(19) . . ?
C33 C34 O41 45.5(13) . . ?
C35 C34 C37 52.0(18) . . ?
C33 C34 C37 125.3(16) . . ?
O41 C34 C37 87(2) . . ?
C35 C34 C32 103.9(19) . . ?
C33 C34 C32 93.7(10) . . ?
O41 C34 C32 92.1(16) . . ?
C37 C34 C32 55.7(13) . . ?
C35 C34 C36 81.6(19) . . ?
C33 C34 C36 61.3(11) . . ?
O41 C34 C36 43.9(15) . . ?
C37 C34 C36 65.1(15) . . ?
C32 C34 C36 48.2(10) . . ?
C34 C35 C37 80(2) . . ?
C34 C35 O41 68(2) . . ?
C37 C35 O41 102(3) . . ?
O41 C36 C32 108(3) . . ?
O41 C36 C33 40.1(17) . . ?
C32 C36 C33 86.6(16) . . ?
O41 C36 C31 112(2) . . ?
C32 C36 C31 45.6(10) . . ?
C33 C36 C31 72.7(13) . . ?
O41 C36 C37 80(2) . . ?
C32 C36 C37 51.2(13) . . ?
C33 C36 C37 92.0(17) . . ?
C31 C36 C37 95.5(17) . . ?
O41 C36 C34 51.5(18) . . ?
C32 C36 C34 56.3(11) . . ?
C33 C36 C34 43.9(9) . . ?
C31 C36 C34 75.3(13) . . ?
C37 C36 C34 48.6(12) . . ?
C35 C37 C32 109(3) . . ?
C35 C37 C34 48.3(18) . . ?
C32 C37 C34 64.7(14) . . ?
C35 C37 C36 81(2) . . ?
C32 C37 C36 49.7(13) . . ?
C34 C37 C36 66.2(16) . . ?
C33 O41 C36 90(3) . . ?
C33 O41 C35 106(3) . . ?
C36 O41 C35 97(3) . . ?
C33 O41 C34 61.1(19) . . ?
C36 O41 C34 85(2) . . ?
C35 O41 C34 47.1(16) . . ?
O211 C211 C220 119.8(4) . . ?
O211 C211 C212 119.4(4) . . ?
C220 C211 C212 120.8(4) . . ?
C213 C212 C211 119.2(4) . . ?
C213 C212 C221 120.8(4) . . ?
C211 C212 C221 119.9(4) . . ?
C212 C213 C214 121.8(4) . . ?
C215 C214 C213 121.8(4) . . ?
C215 C214 C219 119.8(4) . . ?
C213 C214 C219 118.4(4) . . ?
C216 C215 C214 121.6(4) . . ?
C215 C216 C217 119.5(4) . . ?
C218 C217 C216 121.0(4) . . ?
C217 C218 C219 121.4(4) . . ?
C220 C219 C218 122.9(4) . . ?
C220 C219 C214 120.5(4) . . ?
C218 C219 C214 116.6(4) . . ?
C211 C220 C219 119.2(4) . . ?
C211 C220 C222 119.0(4) . . ?
C219 C220 C222 121.7(3) . . ?
O221 C221 O222 124.9(5) . . ?
O221 C221 C212 119.4(4) . . ?
O222 C221 C212 115.6(5) . . ?
C223 C222 C220 115.8(3) . . ?
C224 C223 C232 118.4(3) . . ?
C224 C223 C222 120.7(3) . . ?
C232 C223 C222 120.8(3) . . ?
O224 C224 C223 118.7(3) . . ?
O224 C224 C225 120.2(3) . . ?
C223 C224 C225 121.1(4) . . ?
C226 C225 C224 119.8(4) . . ?
C226 C225 C233 120.5(4) . . ?
C224 C225 C233 119.7(4) . . ?
C225 C226 C227 121.4(4) . . ?
C226 C227 C228 121.3(4) . . ?
C226 C227 C232 118.8(4) . . ?
C228 C227 C232 119.8(4) . . ?
C229 C228 C227 121.1(4) . . ?
C228 C229 C230 120.0(4) . . ?
C231 C230 C229 121.3(4) . . ?
C230 C231 C232 120.4(4) . . ?
C231 C232 C223 122.6(4) . . ?
C231 C232 C227 117.1(4) . . ?
C223 C232 C227 120.2(4) . . ?
O233 C233 O234 124.0(4) . . ?
O233 C233 C225 121.8(4) . . ?
O234 C233 C225 114.2(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N11 C16 1.301(8) . ?
N11 C12 1.432(9) . ?
C12 C13 1.367(10) . ?
C12 C17 1.428(9) . ?
C13 C14 1.301(9) . ?
C14 C15 1.336(10) . ?
C15 C16 1.377(9) . ?
C15 C18 1.473(11) . ?
O31 C31 1.317(14) . ?
O31 C33 1.464(14) . ?
C31 C32 1.338(15) . ?
C31 C36 1.84(3) . ?
C32 C36 1.53(3) . ?
C32 C37 1.56(3) . ?
C32 C34 1.709(19) . ?
C33 O41 1.17(3) . ?
C33 C34 1.430(17) . ?
C33 C36 1.81(3) . ?
C34 C35 1.24(3) . ?
C34 O41 1.56(4) . ?
C34 C37 1.63(4) . ?
C34 C36 1.99(3) . ?
C35 C37 1.31(4) . ?
C35 O41 1.53(4) . ?
C36 O41 1.39(4) . ?
C36 C37 1.97(4) . ?
O211 C211 1.358(5) . ?
C211 C220 1.386(5) . ?
C211 C212 1.446(6) . ?
C212 C213 1.351(6) . ?
C212 C221 1.509(6) . ?
C213 C214 1.416(6) . ?
C214 C215 1.411(6) . ?
C214 C219 1.432(6) . ?
C215 C216 1.347(6) . ?
C216 C217 1.410(6) . ?
C217 C218 1.359(6) . ?
C218 C219 1.431(6) . ?
C219 C220 1.402(6) . ?
C220 C222 1.537(5) . ?
C221 O221 1.245(7) . ?
C221 O222 1.274(6) . ?
C222 C223 1.513(5) . ?
C223 C224 1.383(5) . ?
C223 C232 1.429(6) . ?
C224 O224 1.359(5) . ?
C224 C225 1.429(5) . ?
C225 C226 1.367(6) . ?
C225 C233 1.491(6) . ?
C226 C227 1.397(6) . ?
C227 C228 1.418(6) . ?
C227 C232 1.429(6) . ?
C228 C229 1.347(6) . ?
C229 C230 1.395(7) . ?
C230 C231 1.377(6) . ?
C231 C232 1.426(6) . ?
C233 O233 1.229(5) . ?
C233 O234 1.296(5) . ?
