Biguanide–transition metals complexes as potential drug for hyperglycemia treatment
Villamizar-Delgado, Stephanny; Porras-Osorio, Laura M.; Piñeros, Octavio; Ellena, Javier; Balcazar, Norman; Varela-Miranda, Ruben E.; D'Vries, Richard F.; RSC Advances 10 (2020) 22856–22863; doi:10.1039/D0RA04059B

data_7240747
_publ_section_title
;
 Biguanide--transition metals complexes as potential drug for
 hyperglycemia treatment
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              22856
_journal_page_last               22863
_journal_paper_doi               10.1039/D0RA04059B
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C8 H21 N10 Ni, Cl, H2 O'
_chemical_formula_sum            'C8 H23 Cl N10 Ni O'
_chemical_formula_weight         369.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-27
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-04-23 deposited with the CCDC.	2020-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.757(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3863(6)
_cell_length_b                   14.8373(9)
_cell_length_c                   15.7512(9)
_cell_measurement_reflns_used    4052
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.5560
_cell_measurement_theta_min      2.7290
_cell_volume                     3025.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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    -64.00 118.00   1.00   19.50    --   27.63  54.00 -30.00  182
  2  \w     23.00  59.00   1.00   19.50    --   27.63  54.00-150.00   36
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0103124000
_diffrn_orient_matrix_UB_12      -0.0346910000
_diffrn_orient_matrix_UB_13      0.0276652000
_diffrn_orient_matrix_UB_21      -0.0293701000
_diffrn_orient_matrix_UB_22      -0.0233867000
_diffrn_orient_matrix_UB_23      -0.0373201000
_diffrn_orient_matrix_UB_31      0.0451505000
_diffrn_orient_matrix_UB_32      -0.0230211000
_diffrn_orient_matrix_UB_33      -0.0035044000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.674
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         8724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+2.5740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4991
_reflns_number_total             8724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04059b2.cif
_cod_data_source_block           Ni_metf1
_cod_depositor_comments
;
Adding full bibliography for 7240746--7240749.cif.

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C8 H21 N10 Ni), 2(Cl), 2(H2 O)'
_cod_original_formula_sum        'C16 H46 Cl2 N20 Ni2 O2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     739.05
_cod_database_code               7240747
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ni N15 C12 H33 Cl2'
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.649
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2C,H2D)
2.b Rotating group:
 N2(H2A,H2B), N17(H17A,H17B), N12(H12A,H12B)
2.c X=CH2 refined with riding coordinates:
 N7(H7A,H7B)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12C,H12D,H12E), C4(H4A,H4B,H4C), C15(H15A,H15B,H15C),
 C3(H3A,H3B,H3C), C7(H7C,H7D,H7E), C16(H16A,H16B,H16C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              86191
_olex2_submission_original_sample_id MfnNi1
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.919