#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/56/7205652.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_7205652
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-, C3 H7 N O , C2 H8 N 1+'
_chemical_formula_sum            'C28 H30 N2 O7'
_chemical_formula_weight         506.54
_chemical_name_common            'dimethylammonium 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                 95.5190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8970(9)
_cell_length_b                   13.7462(13)
_cell_length_c                   21.261(2)
_cell_measurement_reflns_used    2834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.309
_cell_measurement_theta_min      2.429
_cell_volume                     2588.2(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 1.000
_diffrn_measured_fraction_theta_max 0.931
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15381
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9898
_exptl_absorpt_correction_T_min  0.9849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0495P)²+0.7284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                3885
_reflns_number_total             5687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00528b.txt
_cod_data_source_block           1g
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7205652
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
O1 O 0.3750(3) 0.35281(16) 0.16751(8) 0.0747(6) Uani 1 1 d . . .
C2 C 0.3531(3) 0.2639(2) 0.17595(12) 0.0558(7) Uani 1 1 d . . .
H2 H 0.2804 0.2315 0.1477 0.067 Uiso 1 1 calc R . .
N3 N 0.4256(2) 0.21297(14) 0.22192(8) 0.0392(5) Uani 1 1 d . . .
C4 C 0.3938(3) 0.11064(17) 0.23096(11) 0.0441(6) Uani 1 1 d . . .
H4A H 0.3173 0.0887 0.1977 0.066 Uiso 1 1 calc R . .
H4B H 0.3561 0.1013 0.2724 0.066 Uiso 1 1 calc R . .
H4C H 0.4865 0.0728 0.2289 0.066 Uiso 1 1 calc R . .
C5 C 0.5429(3) 0.25714(17) 0.26516(10) 0.0440(6) Uani 1 1 d . . .
H5A H 0.6410 0.2289 0.2581 0.066 Uiso 1 1 calc R . .
H5B H 0.5214 0.2449 0.3088 0.066 Uiso 1 1 calc R . .
H5C H 0.5452 0.3274 0.2576 0.066 Uiso 1 1 calc R . .
N11 N 0.31426(18) 0.49015(13) 0.07950(8) 0.0266(4) Uani 1 1 d . . .
H1N H 0.354(2) 0.4882(14) 0.0398(10) 0.030(5) Uiso 1 1 d . . .
H2N H 0.344(2) 0.4324(17) 0.1025(10) 0.042(6) Uiso 1 1 d . . .
C12 C 0.1478(2) 0.49080(17) 0.07045(9) 0.0355(5) Uani 1 1 d . . .
H12A H 0.1075 0.4953 0.1116 0.053 Uiso 1 1 calc R . .
H12B H 0.1119 0.4307 0.0492 0.053 Uiso 1 1 calc R . .
H12C H 0.1134 0.5469 0.0444 0.053 Uiso 1 1 calc R . .
C13 C 0.3755(3) 0.57798(17) 0.11254(10) 0.0432(6) Uani 1 1 d . . .
H13A H 0.3430 0.6358 0.0879 0.065 Uiso 1 1 calc R . .
H13B H 0.4861 0.5748 0.1173 0.065 Uiso 1 1 calc R . .
H13C H 0.3382 0.5817 0.1544 0.065 Uiso 1 1 calc R . .
O211 O 0.44782(13) 0.78196(9) 0.46295(6) 0.0219(3) Uani 1 1 d . . .
H211 H 0.442(2) 0.8493(18) 0.4698(10) 0.046(7) Uiso 1 1 d . . .
C211 C 0.33811(19) 0.76581(12) 0.41449(8) 0.0176(4) Uani 1 1 d . . .
C212 C 0.24669(18) 0.84517(12) 0.38979(8) 0.0179(4) Uani 1 1 d . . .
C213 C 0.13854(19) 0.82861(13) 0.34060(8) 0.0205(4) Uani 1 1 d . . .
H213 H 0.0751 0.8807 0.3252 0.025 Uiso 1 1 calc R . .
C214 C 0.11895(19) 0.73607(13) 0.31214(8) 0.0200(4) Uani 1 1 d . . .
C215 C 0.0139(2) 0.72105(14) 0.25836(8) 0.0242(4) Uani 1 1 d . . .
H215 H -0.0488 0.7733 0.2426 0.029 Uiso 1 1 calc R . .
C216 C 0.0017(2) 0.63281(14) 0.22902(9) 0.0270(4) Uani 1 1 d . . .
H216 H -0.0686 0.6235 0.1930 0.032 Uiso 1 1 calc R . .
C217 C 0.0949(2) 0.55541(13) 0.25291(8) 0.0255(4) Uani 1 1 d . . .
H217 H 0.0877 0.4942 0.2321 0.031 Uiso 1 1 calc R . .
C218 C 0.1953(2) 0.56674(13) 0.30522(8) 0.0213(4) Uani 1 1 d . . .
H218 H 0.2558 0.5131 0.3203 0.026 Uiso 1 1 calc R . .
C219 C 0.21085(19) 0.65738(12) 0.33742(8) 0.0177(4) Uani 1 1 d . . .
C220 C 0.31784(19) 0.67234(12) 0.39107(8) 0.0177(4) Uani 1 1 d . . .
O221 O 0.17279(14) 1.01009(9) 0.39756(6) 0.0238(3) Uani 1 1 d . . .
C221 C 0.2655(2) 0.94518(13) 0.41725(8) 0.0196(4) Uani 1 1 d . . .
O222 O 0.37456(13) 0.95990(9) 0.45955(6) 0.0228(3) Uani 1 1 d . . .
C222 C 0.4140(2) 0.58970(12) 0.42093(8) 0.0187(4) Uani 1 1 d . . .
H22A H 0.4708 0.5602 0.3879 0.022 Uiso 1 1 calc R . .
H22B H 0.4888 0.6176 0.4535 0.022 Uiso 1 1 calc R . .
C223 C 0.32797(19) 0.50937(12) 0.45138(8) 0.0178(4) Uani 1 1 d . . .
O224 O 0.40150(14) 0.39916(9) 0.37492(6) 0.0240(3) Uani 1 1 d . . .
H224 H 0.391(3) 0.3340(19) 0.3656(12) 0.061(8) Uiso 1 1 d . . .
C224 C 0.32678(19) 0.41619(13) 0.42690(8) 0.0195(4) Uani 1 1 d . . .
C225 C 0.24892(19) 0.33816(12) 0.45427(8) 0.0191(4) Uani 1 1 d . . .
C226 C 0.17261(19) 0.35620(13) 0.50633(8) 0.0199(4) Uani 1 1 d . . .
H226 H 0.1190 0.3048 0.5240 0.024 Uiso 1 1 calc R . .
C227 C 0.17250(19) 0.44941(13) 0.53388(8) 0.0192(4) Uani 1 1 d . . .
C228 C 0.0958(2) 0.46797(13) 0.58828(8) 0.0230(4) Uani 1 1 d . . .
H228 H 0.0410 0.4170 0.6058 0.028 Uiso 1 1 calc R . .
C229 C 0.0995(2) 0.55746(14) 0.61574(9) 0.0258(4) Uani 1 1 d . . .
H229 H 0.0475 0.5688 0.6520 0.031 Uiso 1 1 calc R . .
C230 C 0.1808(2) 0.63312(14) 0.59002(8) 0.0248(4) Uani 1 1 d . . .
H230 H 0.1842 0.6953 0.6096 0.030 Uiso 1 1 calc R . .
C231 C 0.2552(2) 0.61877(13) 0.53738(8) 0.0221(4) Uani 1 1 d . . .
H231 H 0.3094 0.6711 0.5210 0.026 Uiso 1 1 calc R . .
C232 C 0.25248(19) 0.52663(12) 0.50669(8) 0.0176(4) Uani 1 1 d . . .
O233 O 0.31277(15) 0.22258(9) 0.37790(6) 0.0295(3) Uani 1 1 d . . .
C233 C 0.2504(2) 0.23981(13) 0.42594(8) 0.0217(4) Uani 1 1 d . . .
O234 O 0.17992(15) 0.17138(9) 0.45482(6) 0.0256(3) Uani 1 1 d . . .
H234 H 0.184(3) 0.1055(19) 0.4305(12) 0.064(8) Uiso 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
O1 C2 N3 123.5(3) . . ?
C2 N3 C4 121.7(2) . . ?
C2 N3 C5 121.1(2) . . ?
C4 N3 C5 117.25(18) . . ?
C13 N11 C12 112.18(17) . . ?
O211 C211 C220 118.74(15) . . ?
O211 C211 C212 119.49(15) . . ?
C220 C211 C212 121.76(15) . . ?
C213 C212 C211 119.10(16) . . ?
C213 C212 C221 119.62(15) . . ?
C211 C212 C221 121.28(15) . . ?
C212 C213 C214 121.69(16) . . ?
C213 C214 C215 121.35(16) . . ?
C213 C214 C219 118.56(15) . . ?
C215 C214 C219 120.06(16) . . ?
C216 C215 C214 120.98(17) . . ?
C215 C216 C217 119.16(17) . . ?
C218 C217 C216 121.45(17) . . ?
C217 C218 C219 121.15(17) . . ?
C218 C219 C220 122.49(16) . . ?
C218 C219 C214 117.16(15) . . ?
C220 C219 C214 120.29(15) . . ?
C211 C220 C219 118.36(15) . . ?
C211 C220 C222 119.59(15) . . ?
C219 C220 C222 121.99(15) . . ?
O221 C221 O222 123.52(16) . . ?
O221 C221 C212 118.44(15) . . ?
O222 C221 C212 118.04(15) . . ?
C223 C222 C220 115.63(14) . . ?
C224 C223 C232 118.46(15) . . ?
C224 C223 C222 119.85(15) . . ?
C232 C223 C222 121.64(15) . . ?
O224 C224 C223 118.52(15) . . ?
O224 C224 C225 119.59(15) . . ?
C223 C224 C225 121.89(15) . . ?
C226 C225 C224 119.20(16) . . ?
C226 C225 C233 121.07(16) . . ?
C224 C225 C233 119.72(15) . . ?
C225 C226 C227 121.25(16) . . ?
C226 C227 C228 121.41(16) . . ?
C226 C227 C232 119.11(15) . . ?
C228 C227 C232 119.48(16) . . ?
C229 C228 C227 121.17(17) . . ?
C228 C229 C230 119.57(17) . . ?
C231 C230 C229 121.23(17) . . ?
C230 C231 C232 121.00(17) . . ?
C231 C232 C223 122.43(16) . . ?
C231 C232 C227 117.51(15) . . ?
C223 C232 C227 120.05(15) . . ?
O233 C233 O234 121.53(16) . . ?
O233 C233 C225 122.35(16) . . ?
O234 C233 C225 116.12(15) . . ?
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
O1 C2 1.253(3) . ?
C2 N3 1.319(3) . ?
N3 C4 1.451(3) . ?
N3 C5 1.455(3) . ?
N11 C13 1.475(3) . ?
N11 C12 1.475(2) . ?
O211 C211 1.368(2) . ?
C211 C220 1.383(2) . ?
C211 C212 1.430(2) . ?
C212 C213 1.370(2) . ?
C212 C221 1.497(2) . ?
C213 C214 1.412(2) . ?
C214 C215 1.421(2) . ?
C214 C219 1.429(2) . ?
C215 C216 1.363(3) . ?
C216 C217 1.413(3) . ?
C217 C218 1.367(2) . ?
C218 C219 1.422(2) . ?
C219 C220 1.429(2) . ?
C220 C222 1.524(2) . ?
O221 C221 1.259(2) . ?
C221 O222 1.274(2) . ?
C222 C223 1.523(2) . ?
C223 C224 1.382(2) . ?
C223 C232 1.429(2) . ?
O224 C224 1.364(2) . ?
C224 C225 1.431(2) . ?
C225 C226 1.376(2) . ?
C225 C233 1.481(2) . ?
C226 C227 1.409(2) . ?
C227 C228 1.422(2) . ?
C227 C232 1.431(2) . ?
C228 C229 1.361(3) . ?
C229 C230 1.407(3) . ?
C230 C231 1.368(3) . ?
C231 C232 1.424(2) . ?
O233 C233 1.232(2) . ?
C233 O234 1.315(2) . ?
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 H2N O1 0.96(2) 1.76(2) 2.676(3) 158.4(19) .
O234 H234 O221 1.05(3) 1.49(3) 2.5272(17) 174(2) 1_545
N11 H1N O222 0.95(2) 1.87(2) 2.743(2) 151.6(18) 4_575
N11 H1N O222 0.95(2) 2.45(2) 2.995(2) 116.8(15) 2_645
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30653752
