Solid-state landscape and biopharmaceutical implications of novel metformin-based salts
Diniz, Luan F.; Carvalho, Paulo S.; Gonçalves, José E.; Diniz, Renata; Fernandes, Christian; New Journal of Chemistry 46 (2022) 13725–13737; doi:10.1039/D2NJ00453D

data_7061640
_publ_section_title
;
 Solid-state landscape and biopharmaceutical implications of novel
 metformin-based salts
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13725
_journal_page_last               13737
_journal_paper_doi               10.1039/D2NJ00453D
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C4 H3 O4, C4 H12 N5'
_chemical_formula_sum            'C8 H15 N5 O4'
_chemical_formula_weight         245.25
_chemical_name_systematic        'Metformin maleate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-05 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.807(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5887(8)
_cell_length_b                   8.8945(5)
_cell_length_c                   13.6358(9)
_cell_measurement_reflns_used    2340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8590
_cell_measurement_theta_min      2.7850
_cell_volume                     1222.71(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4186
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -87.00  15.00   1.00    4.50    --  -11.01 -38.00 120.00  102
  2  \w    -80.00  20.00   1.00    4.50    --  -11.01 -77.00  30.00  100
  3  \w    -37.00  54.00   1.00    4.50    --  -11.01  38.00 -60.00   91
  4  \w    -45.00 -15.00   1.00    4.50    --   13.04 135.00  -3.00   30
  5  \w    -13.00  28.00   1.00    4.50    --   13.04  38.00-180.00   41
  6  \w      3.00  28.00   1.00    4.50    --   13.04  77.00 120.00   25
  7  \w    -36.00 -11.00   1.00    4.50    --   13.04 135.00 176.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0562882000
_diffrn_orient_matrix_UB_12      -0.0065230000
_diffrn_orient_matrix_UB_13      0.0442952000
_diffrn_orient_matrix_UB_21      0.0411477000
_diffrn_orient_matrix_UB_22      -0.0092910000
_diffrn_orient_matrix_UB_23      -0.0319955000
_diffrn_orient_matrix_UB_31      0.0094897000
_diffrn_orient_matrix_UB_32      0.0789125000
_diffrn_orient_matrix_UB_33      -0.0000925000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9856
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.776
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.082(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.4228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1858
_reflns_number_total             2759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00453d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7061640--7061642.cif.'
_cod_database_code               7061640
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2.a Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              11506
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.381
_oxdiff_exptl_absorpt_empirical_full_min 0.846