Synthesis, Characterization and Structural Analysis of Two New Biguanide Complexes
Pastrana-Dávila, Andrea; Minotta, Gianella; Ellena, Javier; Santiago, Pedro H. O.; D’Vries, Richard F.; Crystals 13 (2023) 1176–; doi:10.3390/cryst13081176

data_1569624
_publ_section_title
;
 Synthesis, Characterization and Structural Analysis of Two New Biguanide
 Complexes
;
_journal_issue                   8
_journal_name_full               Crystals
_journal_page_first              1176
_journal_paper_doi               10.3390/cryst13081176
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C4 H11 Cl2 Cu N5'
_chemical_formula_sum            'C4 H11 Cl2 Cu N5'
_chemical_formula_weight         263.62
_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
_audit_creation_date             2023-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.925(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5287(3)
_cell_length_b                   16.5771(4)
_cell_length_c                   7.9737(3)
_cell_measurement_reflns_used    10552
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      34.2480
_cell_measurement_theta_min      2.9800
_cell_volume                     909.64(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -4.00  84.00   0.50    6.00    --   12.91  66.00  10.00  176
  2  \w    -58.00  30.00   0.50    6.00    --   12.91 -66.00-124.00  176
  3  \w    -38.00   2.00   0.50    6.00    --  -12.12 -57.00  90.00   80
  4  \w    -16.00  10.00   0.50    6.00    --  -12.12 -77.00-150.00   52
  5  \w    -16.00  10.00   0.50    6.00    --  -12.12 -77.00  30.00   52
  6  \w     53.00  84.00   0.50    6.00    --   12.91-178.00 -90.00   62
  7  \w    -60.00 -23.00   0.50    6.00    --   12.91 -19.00 -60.00   74
  8  \w    -34.00  16.00   0.50    6.00    --  -12.12  77.00  60.00  100
  9  \w    -38.00  -8.00   0.50    6.00    --  -12.12 -57.00-180.00   60
 10  \w    -60.00 -23.00   0.50    6.00    --   12.91 -19.00   0.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002203000
_diffrn_orient_matrix_UB_12      0.0175547000
_diffrn_orient_matrix_UB_13      0.0810121000
_diffrn_orient_matrix_UB_21      -0.0735927000
_diffrn_orient_matrix_UB_22      -0.0273805000
_diffrn_orient_matrix_UB_23      -0.0027616000
_diffrn_orient_matrix_UB_31      0.0721685000
_diffrn_orient_matrix_UB_32      -0.0278186000
_diffrn_orient_matrix_UB_33      0.0538191000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12829
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.694
_diffrn_reflns_theta_min         2.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0360P)^2^+0.5018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2164
_reflns_number_total             2355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Met-Cu-2.cif
_cod_data_source_block           Met-Cu-2
_cod_database_code               1569624
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C4 H11 N5 Cu Cl2'
_chemical_oxdiff_usercomment     'Amostra Met-Cu-01_Richard D`vries'
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.633
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 H2A, H2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Rotating group:
 N2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N1(H1)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              83099
_shelx_hkl_checksum              55890
_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 0.702