#------------------------------------------------------------------------------
#$Date: 2019-11-14 14:42:34 +0200 (Thu, 14 Nov 2019) $
#$Revision: 227796 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/51/7235107.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_7235107
loop_
_publ_author_name
'Ayoub, Ghada'
'Štrukil, Vjekoslav'
'Fábián, László'
'Mottillo, Cristina'
'Bao, Huizhi'
'Murata, Yasujiro'
'Moores, Audrey'
'Margetić, Davor'
'Eckert-Maksić, Mirjana'
'Friščić, Tomislav'
_publ_section_title
;
 Mechanochemistryvs.solution growth: striking differences in bench
 stability of a cimetidine salt based on a synthetic method
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              7242
_journal_paper_doi               10.1039/C8CE01727A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C10 H17 N6 S, C4 H3 O4'
_chemical_formula_sum            'C14 H20 N6 O4 S'
_chemical_formula_weight         368.41
_chemical_name_common            'cimetidinium fumarate'
_chemical_name_systematic        'cimetidinium fumarate polymorph 2'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2016-04-28T17:49
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
;
2018-08-19 deposited with the CCDC.
2018-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 107.419(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.7700(10)
_cell_length_b                   8.0432(5)
_cell_length_c                   18.9493(10)
_cell_measurement_reflns_used    1138
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.52
_cell_volume                     2002.5(2)
_computing_publication_material  GSAS
_computing_structure_refinement  GSAS
_computing_structure_solution    EXPO2014
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'D2 Phaser'
_diffrn_radiation_polarisn_ratio 0.55
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_colour            powder
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       powder
_exptl_crystal_F_000             776
_exptl_crystal_recrystallization_method
'Obtained by desolvation of the mechanochemically prepared acetonitrile solvate of cimetidinium fumarate'
_pd_calc_method                  'Rietveld Refinement'
_pd_char_particle_morphology     'fine powder'
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        60.0
_pd_meas_2theta_range_min        4.0
_pd_meas_number_of_points        5601
_pd_phase_name                   desolvate
_pd_prep_cool_rate               0
_pd_prep_pressure                100
_pd_prep_temperature             293
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        60.0
_pd_proc_2theta_range_min        4.0
_pd_proc_info_datetime           2016-04-28T17:49:47
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 15 terms.
 Shifted Chebyshev function of 1st kind
      1:    41.7660     2:   -21.3965     3:   2.802910E-02 4:  -0.276950    
      5:    7.87529     6:   -6.32487     7:    1.51969     8:    3.23536    
      9:   -1.84630    10:   0.238221    11:   0.838565    12:    2.05028    
     13:   -1.09679    14:  -0.605747    15:    1.42154    
;
_pd_proc_ls_peak_cutoff          0.00300
_pd_proc_ls_profile_function
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =  818.070 #2(GV)   =    0.000 #3(GW)   =    0.000
 #4(GP)   =    0.000 #5(LX)   =   10.035 #6(LY)   =    0.000
 #7(S/L)  =   0.0277 #8(H/L)  =   0.0359
 #9(trns) =     0.00 #10(shft)=  -2.6182
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.000 #15(L22) =    0.000 #16(L33) =    0.000
 #17(L12) =    0.000 #18(L13) =    0.000 #19(L23) =    0.000
 Peak tails are ignored  where the intensity is below 0.0030 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0835
_pd_proc_ls_prof_wR_expected     0.0969
_pd_proc_ls_prof_wR_factor       0.1095
_pd_proc_number_of_points        5601
_pd_spec_mounting                ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.14
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     160
_refine_ls_number_restraints     134
_refine_ls_R_Fsqd_factor         0.05417
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_refine_ls_weighting_details     1/σ(Yobs)²
_refine_ls_weighting_scheme      sigma
_reflns_d_resolution_high        1.542
_reflns_d_resolution_low         12.567
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_total             1138
_cod_data_source_file            c8ce01727a2.cif
_cod_data_source_block           Compound-1'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (44
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (70
times).

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        2002.48(21)
_cod_database_code               7235107
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y+1/2,-z+1/2
-1 -x,-y,-z
-2 +x+1/2,-y+1/2,+z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
C C1 0.35998(17) 0.85144(27) 1.09736(22) 1.0 Uiso 0.0452(12) 4
N N1 0.33158(14) 1.01381(20) 1.10133(21) 1.0 Uiso 0.0452(12) 4
H H1 0.36335(19) 1.09725(27) 1.09308(26) 1.0 Uiso 0.0904(23) 4
C C2 0.28872(15) 0.75589(29) 1.11422(21) 1.0 Uiso 0.0452(12) 4
N N2 0.21984(12) 0.86327(25) 1.12769(18) 1.0 Uiso 0.0452(12) 4
H H2 0.16854(16) 0.84098(34) 1.13918(19) 1.0 Uiso 0.0904(23) 4
C C3 0.24756(14) 1.01856(20) 1.11961(23) 1.0 Uiso 0.0452(12) 4
H H3 0.21214(20) 1.11613(26) 1.12586(29) 1.0 Uiso 0.0904(23) 4
C C4 0.45346(13) 0.80722(17) 1.07746(8) 1.0 Uiso 0.0452(12) 4
H H4A 0.51335(17) 0.8210(5) 1.12084(13) 1.0 Uiso 0.0904(23) 4
H H4B 0.45959(24) 0.87998(32) 1.03753(12) 1.0 Uiso 0.0904(23) 4
H H4C 0.44914(24) 0.69129(22) 1.06089(19) 1.0 Uiso 0.0904(23) 4
C C5 0.28048(12) 0.57309(26) 1.11879(8) 1.0 Uiso 0.0452(12) 4
H H5A 0.28206(26) 0.5425(4) 1.16978(10) 1.0 Uiso 0.0904(23) 4
H H5B 0.34031(15) 0.5213(4) 1.10880(17) 1.0 Uiso 0.0904(23) 4
S S1 0.16490(21) 0.4884(5) 1.05416(20) 1.0 Uiso 0.0452(12) 4
C C6 0.18769(11) 0.52592(21) 0.96583(11) 1.0 Uiso 0.0452(12) 4
H H6A 0.12205(15) 0.5494(4) 0.92793(16) 1.0 Uiso 0.0904(23) 4
H H6B 0.23155(18) 0.62522(26) 0.97005(21) 1.0 Uiso 0.0904(23) 4
C C7 0.23823(11) 0.37938(20) 0.94103(11) 1.0 Uiso 0.0452(12) 4
H H7A 0.30613(14) 0.3612(4) 0.97709(16) 1.0 Uiso 0.0904(23) 4
H H7B 0.19687(18) 0.27832(25) 0.94054(20) 1.0 Uiso 0.0904(23) 4
N N3 0.24989(17) 0.40324(29) 0.86812(11) 1.0 Uiso 0.0452(12) 4
H H4 0.21434(22) 0.3427(4) 0.83330(14) 1.0 Uiso 0.0904(23) 4
C C8 0.32335(20) 0.4981(4) 0.85656(13) 1.0 Uiso 0.0452(12) 4
N N4 0.33019(15) 0.51474(27) 0.78778(12) 1.0 Uiso 0.0452(12) 4
H H5 0.37101(21) 0.5834(4) 0.78029(15) 1.0 Uiso 0.0904(23) 4
C C9 0.26295(10) 0.43653(18) 0.72321(8) 1.0 Uiso 0.0452(12) 4
H H9A 0.25766(27) 0.31765(21) 0.73280(19) 1.0 Uiso 0.0904(23) 4
H H9B 0.28988(21) 0.4511(5) 0.68119(10) 1.0 Uiso 0.0904(23) 4
H H9C 0.19530(14) 0.4876(4) 0.71170(20) 1.0 Uiso 0.0904(23) 4
N N5 0.38706(24) 0.5706(7) 0.91583(18) 1.0 Uiso 0.0452(12) 4
C C10 0.4617(4) 0.6638(8) 0.90779(17) 1.0 Uiso 0.0452(12) 4
N N6 0.5301(5) 0.7478(10) 0.90831(31) 1.0 Uiso 0.0452(12) 4
O O1 0.3631(5) 0.7319(5) 1.3018(4) 1.0 Uiso 0.0208(17) 4
O O2 0.50527(17) 0.62046(27) 1.28581(29) 1.0 Uiso 0.0208(17) 4
H H6 0.47560(23) 0.53041(27) 1.28808(35) 1.0 Uiso 0.0416(35) 4
C C11 0.44575(17) 0.74732(32) 1.29188(30) 1.0 Uiso 0.0208(17) 4
C C12 0.49243(12) 0.91138(29) 1.28742(20) 1.0 Uiso 0.0208(17) 4
H H12 0.55755(15) 0.9163(4) 1.27979(22) 1.0 Uiso 0.0416(35) 4
C C13 0.44554(12) 1.04984(30) 1.29366(20) 1.0 Uiso 0.0208(17) 4
H H13 0.38079(15) 1.0412(4) 1.30158(22) 1.0 Uiso 0.0416(35) 4
C C14 0.48673(19) 1.22035(34) 1.28966(32) 1.0 Uiso 0.0208(17) 4
O O3 0.5694(5) 1.2368(5) 1.2795(4) 1.0 Uiso 0.0208(17) 4
O O4 0.4318(4) 1.3367(6) 1.2976(4) 1.0 Uiso 0.0208(17) 4
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 56.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
N 24.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
H 80.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081
57.7997 0.00304 International_Tables_Vol_C
S 4.0 0.000 0.000 6.90530 1.46790 5.20340 22.2151 1.43790 0.25360 1.58630
56.1720 0.86690 International_Tables_Vol_C
O 16.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
loop_
_diffrn_radiation_wavelength
_diffrn_radiation_wavelength_wt
_diffrn_radiation_wavelength_id
1.540600 1.000 1
1.544400 0.500 2
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
N1 C1 C2 106.75(19) 1_555 1_555 n
N1 C1 C4 121.58(18) 1_555 1_555 n
C2 C1 C4 131.68(16) 1_555 1_555 n
C1 N1 H1 125.23(26) 1_555 1_555 n
C1 N1 C3 109.43(16) 1_555 1_555 n
H1 N1 C3 125.33(22) 1_555 1_555 n
C1 C2 N2 106.14(16) 1_555 1_555 n
C1 C2 C5 130.54(18) 1_555 1_555 n
N2 C2 C5 123.32(18) 1_555 1_555 n
C2 N2 H2 127.98(21) 1_555 1_555 n
C2 N2 C3 109.54(18) 1_555 1_555 n
H2 N2 C3 122.48(22) 1_555 1_555 n
N1 C3 N2 108.15(15) 1_555 1_555 n
N1 C3 H3 125.94(23) 1_555 1_555 n
N2 C3 H3 125.91(26) 1_555 1_555 n
C1 C4 H4A 109.53(20) 1_555 1_555 n
C1 C4 H4B 109.49(20) 1_555 1_555 n
C1 C4 H4C 109.52(20) 1_555 1_555 n
H4A C4 H4B 109.54(22) 1_555 1_555 n
H4A C4 H4C 109.35(23) 1_555 1_555 n
H4B C4 H4C 109.39(23) 1_555 1_555 n
C2 C5 H5A 108.90(22) 1_555 1_555 n
C2 C5 H5B 108.92(19) 1_555 1_555 n
C2 C5 S1 113.50(15) 1_555 1_555 n
H5A C5 H5B 107.76(23) 1_555 1_555 n
H5A C5 S1 108.78(20) 1_555 1_555 n
H5B C5 S1 108.82(19) 1_555 1_555 n
C5 S1 C6 101.51(16) 1_555 1_555 n
S1 C6 H6A 109.14(20) 1_555 1_555 n
S1 C6 H6B 109.21(22) 1_555 1_555 n
S1 C6 C7 112.25(15) 1_555 1_555 n
H6A C6 H6B 107.87(22) 1_555 1_555 n
H6A C6 C7 109.17(20) 1_555 1_555 n
H6B C6 C7 109.10(18) 1_555 1_555 n
C6 C7 H7A 109.13(20) 1_555 1_555 n
C6 C7 H7B 108.98(18) 1_555 1_555 n
C6 C7 N3 112.65(14) 1_555 1_555 n
H7A C7 H7B 107.86(22) 1_555 1_555 n
H7A C7 N3 109.03(20) 1_555 1_555 n
H7B C7 N3 109.08(22) 1_555 1_555 n
C7 N3 H4 117.55(22) 1_555 1_555 n
C7 N3 C8 122.46(15) 1_555 1_555 n
H4 N3 C8 119.29(22) 1_555 1_555 n
N3 C8 N4 119.54(16) 1_555 1_555 n
N3 C8 N5 116.77(20) 1_555 1_555 n
N4 C8 N5 123.68(20) 1_555 1_555 n
C8 N4 H5 118.73(21) 1_555 1_555 n
C8 N4 C9 124.60(16) 1_555 1_555 n
H5 N4 C9 116.22(22) 1_555 1_555 n
N4 C9 H9A 109.48(19) 1_555 1_555 n
N4 C9 H9B 109.54(18) 1_555 1_555 n
N4 C9 H9C 109.43(20) 1_555 1_555 n
H9A C9 H9B 109.53(25) 1_555 1_555 n
H9A C9 H9C 109.35(22) 1_555 1_555 n
H9B C9 H9C 109.50(23) 1_555 1_555 n
C8 N5 C10 119.36(25) 1_555 1_555 n
N5 C10 N6 173.15(33) 1_555 1_555 n
H6 O2 C11 109.54(31) 1_555 1_555 n
O1 C11 O2 124.30(22) 1_555 1_555 n
O1 C11 C12 122.86(22) 1_555 1_555 n
O2 C11 C12 112.82(21) 1_555 1_555 n
C11 C12 H12 119.42(22) 1_555 1_555 n
C11 C12 C13 121.19(18) 1_555 1_555 n
H12 C12 C13 119.39(21) 1_555 1_555 n
C12 C13 H13 117.61(21) 1_555 1_555 n
C12 C13 C14 124.79(18) 1_555 1_555 n
H13 C13 C14 117.60(22) 1_555 1_555 n
C13 C14 O3 119.65(22) 1_555 1_555 n
C13 C14 O4 115.55(27) 1_555 1_555 n
O3 C14 O4 124.79(26) 1_555 1_555 n
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
C1 N1 1.3717(28) 1_555 n
C1 C2 1.3576(34) 1_555 n
C1 C4 1.4889(31) 1_555 n
N1 H1 0.8410(21) 1_555 n
N1 C3 1.3038(35) 1_555 n
C2 N2 1.3622(31) 1_555 n
C2 C5 1.4792(30) 1_555 n
N2 H2 0.8190(22) 1_555 n
N2 C3 1.3282(27) 1_555 n
C3 H3 0.9500(21) 1_555 n
C4 H4A 0.9810(17) 1_555 n
C4 H4B 0.9800(19) 1_555 n
C4 H4C 0.9800(17) 1_555 n
C5 H5A 0.9909(18) 1_555 n
C5 H5B 0.9909(20) 1_555 n
C5 S1 1.8248(32) 1_555 n
S1 C6 1.818(4) 1_555 n
C6 H6A 0.9899(17) 1_555 n
C6 H6B 0.9900(18) 1_555 n
C6 C7 1.5134(25) 1_555 n
C7 H7A 0.9900(17) 1_555 n
C7 H7B 0.9910(18) 1_555 n
C7 N3 1.4504(29) 1_555 n
N3 H4 0.8480(21) 1_555 n
N3 C8 1.3365(34) 1_555 n
C8 N4 1.3413(33) 1_555 n
C8 N5 1.335(4) 1_555 n
N4 H5 0.8300(22) 1_555 n
N4 C9 1.4393(23) 1_555 n
C9 H9A 0.9800(17) 1_555 n
C9 H9B 0.9810(19) 1_555 n
C9 H9C 0.9809(17) 1_555 n
N5 C10 1.317(6) 1_555 n
C10 N6 1.158(8) 1_555 n
O1 C11 1.215(7) 1_555 n
O2 H6 0.8390(22) 1_555 n
O2 C11 1.335(4) 1_555 n
C11 C12 1.4813(34) 1_555 n
C12 H12 0.9509(21) 1_555 n
C12 C13 1.3103(32) 1_555 n
C13 H13 0.9499(21) 1_555 n
C13 C14 1.495(4) 1_555 n
C14 O3 1.217(7) 1_555 n
C14 O4 1.241(6) 1_555 n
loop_
_pd_meas_counts_total
_pd_proc_ls_weight
_pd_proc_intensity_bkg_calc
_pd_calc_intensity_total
90.0 0.01108 73.58623 73.58605
63.0 0.01602 73.54173 73.54156
73.0 0.01384 73.49799 73.49783
76.0 0.01321 73.45500 73.45485
76.0 0.01321 73.41274 73.41259
81.0 0.01235 73.37119 73.37104
75.0 0.01321 73.33033 73.33018
82.0 0.01208 73.29013 73.28999
66.0 0.01524 73.25059 73.25046
86.0 0.01156 73.21168 73.21155
83.0 0.01208 73.17338 73.17326
68.0 0.01487 73.13568 73.13556
76.0 0.01321 73.09856 73.09844
78.0 0.01291 73.06199 73.06188
82.0 0.01208 73.02597 73.02586
67.0 0.01487 72.99048 72.99038
75.0 0.01321 72.95550 72.95540
69.0 0.01452 72.92101 72.92091
72.0 0.01384 72.88699 72.88690
71.0 0.01417 72.85344 72.85336
66.0 0.01524 72.82033 72.82025
71.0 0.01417 72.78765 72.78757
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32.0 . . .
