#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/56/7205641.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_7205641
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         'C23 H15 O6 1- , C7 H10 N 1+ , C3 H7 N O'
_chemical_formula_sum            'C33 H32 N2 O7'
_chemical_formula_weight         568.61
_chemical_name_common            '3,5 lutidinium pamoate DMF 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                 111.3370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8721(11)
_cell_length_b                   12.9708(10)
_cell_length_c                   16.9195(14)
_cell_measurement_reflns_used    5306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.783
_cell_measurement_theta_min      2.267
_cell_volume                     2835.7(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.908
_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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16925
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0609P)²+1.0367P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                4881
_reflns_number_total             6243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00528b.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7205641
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
N1 N -0.44876(10) 0.51577(10) 0.41083(8) 0.0253(3) Uani 1 1 d . . .
O2 O -0.37638(9) 0.39183(9) 0.51014(7) 0.0344(3) Uani 1 1 d . . .
C3 C -0.44648(12) 0.42430(12) 0.44594(10) 0.0261(3) Uani 1 1 d . . .
H3 H -0.5035 0.3797 0.4197 0.031 Uiso 1 1 calc R . .
C4 C -0.53771(13) 0.54801(14) 0.33774(10) 0.0317(4) Uani 1 1 d . . .
H4A H -0.5859 0.4901 0.3179 0.048 Uiso 1 1 calc R . .
H4C H -0.5145 0.5702 0.2922 0.048 Uiso 1 1 calc R . .
H4B H -0.5726 0.6054 0.3539 0.048 Uiso 1 1 calc R . .
C5 C -0.36685(15) 0.59029(15) 0.44693(13) 0.0475(5) Uani 1 1 d . . .
H5C H -0.3915 0.6457 0.4741 0.071 Uiso 1 1 calc R . .
H5B H -0.3464 0.6193 0.4019 0.071 Uiso 1 1 calc R . .
H5A H -0.3072 0.5564 0.4892 0.071 Uiso 1 1 calc R . .
N11 N -0.31690(12) 0.20452(11) 0.58220(9) 0.0339(3) Uani 1 1 d . . .
H11 H -0.3509(17) 0.2618(18) 0.5510(14) 0.053(6) Uiso 1 1 d . . .
C12 C -0.23017(15) 0.17011(13) 0.57435(10) 0.0339(4) Uani 1 1 d . . .
H12 H -0.2071 0.1992 0.5328 0.041 Uiso 1 1 calc R . .
C13 C -0.17339(13) 0.09139(12) 0.62706(10) 0.0291(4) Uani 1 1 d . . .
C14 C -0.21263(13) 0.05209(12) 0.68544(10) 0.0283(4) Uani 1 1 d . . .
H14 H -0.1762 -0.0020 0.7220 0.034 Uiso 1 1 calc R . .
C15 C -0.30366(13) 0.08912(12) 0.69239(10) 0.0310(4) Uani 1 1 d . . .
C16 C -0.35438(14) 0.16740(13) 0.63881(11) 0.0341(4) Uani 1 1 d . . .
H16 H -0.4162 0.1952 0.6420 0.041 Uiso 1 1 calc R . .
C17 C -0.07445(15) 0.05293(15) 0.62147(13) 0.0445(5) Uani 1 1 d . . .
H17B H -0.0164 0.0724 0.6730 0.067 Uiso 1 1 calc R . .
H17A H -0.0648 0.0835 0.5719 0.067 Uiso 1 1 calc R . .
H17C H -0.0772 -0.0223 0.6159 0.067 Uiso 1 1 calc R . .
C18 C -0.34542(17) 0.04786(16) 0.75688(13) 0.0471(5) Uani 1 1 d . . .
H18A H -0.4098 0.0838 0.7510 0.071 Uiso 1 1 calc R . .
H18B H -0.2945 0.0591 0.8141 0.071 Uiso 1 1 calc R . .
H18C H -0.3591 -0.0261 0.7475 0.071 Uiso 1 1 calc R . .
O211 O -0.02880(8) 0.32604(8) 0.40264(6) 0.0212(2) Uani 1 1 d . . .
H211 H -0.0891(18) 0.3169(17) 0.4160(13) 0.054(6) Uiso 1 1 d . . .
C211 C -0.04610(10) 0.26258(10) 0.33496(8) 0.0167(3) Uani 1 1 d . . .
C212 C -0.14107(10) 0.20583(11) 0.30240(8) 0.0166(3) Uani 1 1 d . . .
C213 C -0.16013(10) 0.14443(11) 0.23254(9) 0.0171(3) Uani 1 1 d . . .
H213 H -0.2227 0.1060 0.2116 0.021 Uiso 1 1 calc R . .
C214 C -0.08876(10) 0.13707(10) 0.19096(8) 0.0165(3) Uani 1 1 d . . .
C215 C -0.11284(11) 0.07972(11) 0.11502(9) 0.0191(3) Uani 1 1 d . . .
H215 H -0.1768 0.0439 0.0929 0.023 Uiso 1 1 calc R . .
C216 C -0.04527(11) 0.07525(11) 0.07314(9) 0.0203(3) Uani 1 1 d . . .
H216 H -0.0621 0.0364 0.0223 0.024 Uiso 1 1 calc R . .
C217 C 0.04962(11) 0.12865(11) 0.10587(9) 0.0199(3) Uani 1 1 d . . .
H217 H 0.0965 0.1252 0.0767 0.024 Uiso 1 1 calc R . .
C218 C 0.07545(10) 0.18533(11) 0.17894(9) 0.0175(3) Uani 1 1 d . . .
H218 H 0.1399 0.2205 0.1996 0.021 Uiso 1 1 calc R . .
C219 C 0.00688(10) 0.19233(10) 0.22449(8) 0.0155(3) Uani 1 1 d . . .
C220 C 0.02875(10) 0.25401(10) 0.29872(8) 0.0158(3) Uani 1 1 d . . .
C221 C -0.21980(10) 0.21543(11) 0.34335(9) 0.0181(3) Uani 1 1 d . . .
O221 O -0.20176(8) 0.26812(9) 0.40860(6) 0.0253(2) Uani 1 1 d . . .
O222 O -0.30530(7) 0.16708(8) 0.30579(6) 0.0221(2) Uani 1 1 d . . .
H222 H -0.3687(19) 0.175(2) 0.3384(14) 0.074(8) Uiso 1 1 d . . .
C222 C 0.12909(10) 0.31497(11) 0.33566(8) 0.0171(3) Uani 1 1 d . . .
H22A H 0.1237 0.3609 0.3806 0.021 Uiso 1 1 calc R . .
H22B H 0.1358 0.3595 0.2904 0.021 Uiso 1 1 calc R . .
C223 C 0.22776(10) 0.25149(10) 0.37307(9) 0.0166(3) Uani 1 1 d . . .
O224 O 0.28774(8) 0.31874(8) 0.26863(6) 0.0210(2) Uani 1 1 d . . .
H224 H 0.3460(18) 0.3078(17) 0.2535(14) 0.053(6) Uiso 1 1 d . . .
C224 C 0.30324(10) 0.25685(10) 0.33741(8) 0.0164(3) Uani 1 1 d . . .
C225 C 0.39791(10) 0.19967(10) 0.37192(9) 0.0168(3) Uani 1 1 d . . .
C226 C 0.41417(10) 0.13868(11) 0.44201(9) 0.0175(3) Uani 1 1 d . . .
H226 H 0.4765 0.1001 0.4644 0.021 Uiso 1 1 calc R . .
C227 C 0.34061(10) 0.13194(10) 0.48156(8) 0.0169(3) Uani 1 1 d . . .
C228 C 0.35903(11) 0.07009(11) 0.55508(9) 0.0207(3) Uani 1 1 d . . .
H228 H 0.4205 0.0301 0.5767 0.025 Uiso 1 1 calc R . .
C229 C 0.28915(12) 0.06764(12) 0.59505(9) 0.0229(3) Uani 1 1 d . . .
H229 H 0.3015 0.0253 0.6435 0.027 Uiso 1 1 calc R . .
C230 C 0.19854(11) 0.12854(11) 0.56372(9) 0.0216(3) Uani 1 1 d . . .
H230 H 0.1514 0.1286 0.5927 0.026 Uiso 1 1 calc R . .
C231 C 0.17767(11) 0.18733(11) 0.49238(9) 0.0189(3) Uani 1 1 d . . .
H231 H 0.1158 0.2268 0.4722 0.023 Uiso 1 1 calc R . .
C232 C 0.24717(10) 0.19044(10) 0.44772(8) 0.0165(3) Uani 1 1 d . . .
C233 C 0.47880(11) 0.20784(11) 0.33243(9) 0.0183(3) Uani 1 1 d . . .
O233 O 0.45956(8) 0.25597(9) 0.26458(7) 0.0254(2) Uani 1 1 d . . .
O234 O 0.56527(8) 0.16374(8) 0.37296(6) 0.0234(2) 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 N1 C5 121.54(14) . . ?
C3 N1 C4 120.94(13) . . ?
C5 N1 C4 117.37(14) . . ?
O2 C3 N1 125.60(15) . . ?
C12 N11 C16 123.47(15) . . ?
N11 C12 C13 120.05(16) . . ?
C14 C13 C12 116.59(16) . . ?
C14 C13 C17 121.98(16) . . ?
C12 C13 C17 121.42(17) . . ?
C13 C14 C15 122.36(15) . . ?
C16 C15 C14 117.46(16) . . ?
C16 C15 C18 120.07(17) . . ?
C14 C15 C18 122.46(17) . . ?
N11 C16 C15 120.05(17) . . ?
O211 C211 C220 119.29(12) . . ?
O211 C211 C212 119.40(12) . . ?
C220 C211 C212 121.31(12) . . ?
C213 C212 C211 119.51(12) . . ?
C213 C212 C221 120.27(12) . . ?
C211 C212 C221 120.21(12) . . ?
C212 C213 C214 121.32(12) . . ?
C213 C214 C215 120.77(12) . . ?
C213 C214 C219 119.06(12) . . ?
C215 C214 C219 120.11(12) . . ?
C216 C215 C214 120.88(13) . . ?
C215 C216 C217 119.59(13) . . ?
C218 C217 C216 121.24(13) . . ?
C217 C218 C219 120.95(13) . . ?
C220 C219 C218 122.75(12) . . ?
C220 C219 C214 119.99(12) . . ?
C218 C219 C214 117.22(12) . . ?
C211 C220 C219 118.70(12) . . ?
C211 C220 C222 119.71(12) . . ?
C219 C220 C222 121.50(12) . . ?
O221 C221 O222 123.90(12) . . ?
O221 C221 C212 120.77(12) . . ?
O222 C221 C212 115.32(12) . . ?
C220 C222 C223 116.01(11) . . ?
C224 C223 C232 118.82(12) . . ?
C224 C223 C222 119.89(12) . . ?
C232 C223 C222 121.19(12) . . ?
O224 C224 C223 119.37(12) . . ?
O224 C224 C225 119.22(12) . . ?
C223 C224 C225 121.41(12) . . ?
C226 C225 C224 119.17(12) . . ?
C226 C225 C233 120.61(12) . . ?
C224 C225 C233 120.22(12) . . ?
C225 C226 C227 121.65(13) . . ?
C226 C227 C228 121.22(13) . . ?
C226 C227 C232 118.92(12) . . ?
C228 C227 C232 119.84(12) . . ?
C229 C228 C227 120.70(13) . . ?
C228 C229 C230 119.63(13) . . ?
C231 C230 C229 121.08(13) . . ?
C230 C231 C232 121.14(13) . . ?
C231 C232 C227 117.53(12) . . ?
C231 C232 C223 122.49(12) . . ?
C227 C232 C223 119.96(12) . . ?
O233 C233 O234 124.17(13) . . ?
O233 C233 C225 119.98(12) . . ?
O234 C233 C225 115.85(12) . . ?
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
N1 C3 1.322(2) . ?
N1 C5 1.447(2) . ?
N1 C4 1.4547(19) . ?
O2 C3 1.2387(19) . ?
N11 C12 1.335(2) . ?
N11 C16 1.335(2) . ?
C12 C13 1.395(2) . ?
C13 C14 1.387(2) . ?
C13 C17 1.495(3) . ?
C14 C15 1.395(2) . ?
C15 C16 1.372(2) . ?
C15 C18 1.507(3) . ?
O211 C211 1.3589(17) . ?
C211 C220 1.3890(18) . ?
C211 C212 1.4329(19) . ?
C212 C213 1.3689(19) . ?
C212 C221 1.4962(18) . ?
C213 C214 1.4112(18) . ?
C214 C215 1.4153(19) . ?
C214 C219 1.4312(19) . ?
C215 C216 1.367(2) . ?
C216 C217 1.410(2) . ?
C217 C218 1.369(2) . ?
C218 C219 1.4285(18) . ?
C219 C220 1.4255(19) . ?
C220 C222 1.5233(18) . ?
C221 O221 1.2440(17) . ?
C221 O222 1.2866(17) . ?
C222 C223 1.5236(18) . ?
C223 C224 1.3874(18) . ?
C223 C232 1.4309(19) . ?
O224 C224 1.3647(17) . ?
C224 C225 1.4344(19) . ?
C225 C226 1.374(2) . ?
C225 C233 1.5040(18) . ?
C226 C227 1.4119(18) . ?
C227 C228 1.423(2) . ?
C227 C232 1.4295(19) . ?
C228 C229 1.369(2) . ?
C229 C230 1.414(2) . ?
C230 C231 1.367(2) . ?
C231 C232 1.4256(19) . ?
C233 O233 1.2474(17) . ?
C233 O234 1.2798(17) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11 O2 0.93(2) 1.81(2) 2.7088(19) 161(2) .
O222 H222 O234 1.20(2) 1.26(2) 2.4499(14) 169(2) 1_455
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30653749
