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_7235107
_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/\s(Y~obs~)^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