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_1569625
_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         'C12 H33 Co N15, Cl4.008 Co, Cl, 3(H2 O)'
_chemical_formula_sum            'C12 H39 Cl5.01 Co2 N15 O3'
_chemical_formula_weight         736.96
_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                 101.374(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3808(2)
_cell_length_b                   26.2761(5)
_cell_length_c                   11.3407(3)
_cell_measurement_reflns_used    18545
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      34.0260
_cell_measurement_theta_min      2.5230
_cell_volume                     3032.62(12)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     28.00  78.00   0.50   42.00    --   12.91-155.00 -50.00  100
  2  \w    -16.00  10.00   0.50   42.00    --  -12.12 -77.00  30.00   52
  3  \w     53.00  84.00   0.50   42.00    --   12.91-178.00-150.00   62
  4  \w    -60.00 -23.00   0.50   42.00    --   12.91 -19.00 150.00   74
  5  \w    -60.00 -23.00   0.50   42.00    --   12.91 -19.00-120.00   74
  6  \w    -16.00  35.00   0.50   42.00    --   12.91 -77.00   0.00  102
  7  \w     -1.00  38.00   0.50   42.00    --   12.91  57.00 120.00   78
  8  \w    -60.00 -23.00   0.50   42.00    --   12.91 -19.00 120.00   74
  9  \w    -16.00  35.00   0.50   42.00    --   12.91 -77.00-150.00  102
 10  \w     -1.00  38.00   0.50   42.00    --   12.91  57.00-120.00   78
 11  \w     -1.00  38.00   0.50   42.00    --   12.91  57.00  60.00   78
 12  \w    -60.00 -35.00   0.50   42.00    --   12.91 -19.00  60.00   50
;
_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      -0.0322744000
_diffrn_orient_matrix_UB_12      0.0229977000
_diffrn_orient_matrix_UB_13      -0.0210915000
_diffrn_orient_matrix_UB_21      -0.0583041000
_diffrn_orient_matrix_UB_22      -0.0137965000
_diffrn_orient_matrix_UB_23      -0.0228616000
_diffrn_orient_matrix_UB_31      -0.0204133000
_diffrn_orient_matrix_UB_32      0.0030402000
_diffrn_orient_matrix_UB_33      0.0557082000
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43679
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83806
_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            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1517
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0137P)^2^+3.8340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6560
_reflns_number_total             7831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Met-Co-2.cif
_cod_data_source_block           Met-Co-2
_cod_database_code               1569625
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C4 H11 N5 Co Cl2'
_chemical_oxdiff_usercomment     'Amostra Met-Co-01_Richard D`vries'
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.871
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl5(0.8537) Cl6(0.15415)
3.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12C,H12D,H12E),
 C7(H7C,H7D,H7E), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              71720
_shelx_hkl_checksum              16570
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.875