Mechanochemistryvs.solution growth: striking differences in bench stability of a cimetidine salt based on a synthetic method
Ayoub, Ghada; Štrukil, Vjekoslav; Fábián, László; Mottillo, Cristina; Bao, Huizhi; Murata, Yasujiro; Moores, Audrey; Margetić, Davor; Eckert-Maksić, Mirjana; Friščić, Tomislav; CrystEngComm 20 (2018) 7242–; doi:10.1039/C8CE01727A

data_7235106
_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 1'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2017-08-03T17:38
_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                87.6100(33)
_cell_angle_beta                 75.2582(30)
_cell_angle_gamma                76.179(5)
_cell_formula_units_Z            2
_cell_length_a                   7.90643(32)
_cell_length_b                   8.3568(4)
_cell_length_c                   14.2156(5)
_cell_measurement_reflns_used    1012
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.22
_cell_volume                     881.86(7)
_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_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    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       powder
_exptl_crystal_F_000             388
_exptl_crystal_recrystallization_method
'Mechanochemical synthesis by liquid-assisted grinding in presence of water'
_pd_block_id                     2017-08-03T17:38|R3|L_Fabian|UNK
_pd_calc_method                  'Rietveld Refinement'
_pd_char_particle_morphology     'fine powder'
_pd_instr_location               ' ?'
_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                   'cim-fum H2O'
_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           2017-08-03T17:38:17
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 10 terms.
 Shifted Chebyshev function of 1st kind
      1:    38.2723     2:   -17.2687     3:    2.69286     4:   -5.60365    
      5:    8.20080     6:   -5.19617     7:  -0.263841     8:    1.03178    
      9:  -0.475935    10:  -0.448916    
;
_pd_proc_ls_peak_cutoff          0.00300
_pd_proc_ls_pref_orient_corr
;   March-Dollase
 AXIS  1 Ratio=     1.072 Frac     0.560  h= 2.000  k= 1.000  l= 2.000
 AXIS  2 Ratio=     0.953 Frac     0.440  h= 1.000  k= 1.000  l= 4.000
 Prefered orientation correction range: Min=   0.89418, Max=   1.08645
;
_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)   =  197.376 #2(GV)   =    0.000 #3(GW)   =    2.704
 #4(GP)   =    0.000 #5(LX)   =    2.780 #6(LY)   =   13.012
 #7(S/L)  =   0.0249 #8(H/L)  =   0.0403
 #9(trns) =     0.00 #10(shft)=   1.3401
 #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        0.0976
_pd_proc_ls_prof_wR_expected     0.1039
_pd_proc_ls_prof_wR_factor       0.1315
_pd_proc_number_of_points        5601
_pd_spec_mounting                ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.41
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     151
_refine_ls_number_restraints     134
_refine_ls_R_Fsqd_factor         0.08581
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.01
_refine_ls_weighting_details     1/\s(Y~obs~)^2^
_refine_ls_weighting_scheme      sigma
_reflns_d_resolution_high        1.540
_reflns_d_resolution_low         13.745
_reflns_limit_h_max              5
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              -5
_reflns_limit_l_max              9
_reflns_limit_l_min              -9
_reflns_number_total             1012
_cod_data_source_file            c8ce01727a2.cif
_cod_data_source_block           Compound-2
_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        881.86(6)
_cod_database_code               7235106
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000