Comparison of structural, spectroscopic, theoretical and thermal properties of metal complexes (Zn(II), Mn(II), Cu(II), Ni(II) and Co(II)) of pyridazine-3-carboxylic acid and pyridazine-4-carboxylic acids
Świderski, Grzegorz; Łyszczek, Renata; Wojtulewski, Sławomir; Kalinowska, Monika; Świsłocka, Renata; Lewandowski, Włodzimierz; Inorganica Chimica Acta 512 (2020) 119865–; doi:10.1016/j.ica.2020.119865

data_1564076
_publ_section_title
;
 Comparison of structural, spectroscopic, theoretical and thermal
 properties of metal complexes (Zn(II), Mn(II), Cu(II), Ni(II) and Co(II))
 of pyridazine-3-carboxylic acid and pyridazine-4-carboxylic acids
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119865
_journal_paper_doi               10.1016/j.ica.2020.119865
_journal_volume                  512
_journal_year                    2020
_chemical_formula_moiety         'C10 H14 Mn N4 O8, 2(H2 O)'
_chemical_formula_sum            'C10 H18 Mn N4 O10'
_chemical_formula_weight         409.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.344(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.1170(10)
_cell_length_b                   6.7745(3)
_cell_length_c                   6.2323(4)
_cell_measurement_reflns_used    4033
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.1890
_cell_measurement_theta_min      4.6720
_cell_volume                     800.51(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4052
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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    -11.00  38.00   1.00    1.00    --   43.67  77.00 -90.00   49
  2  \w     49.00 107.00   1.00    1.00    --   43.67  77.00 -90.00   58
  3  \w    112.00 150.00   1.00    1.00    --   43.67  77.00 -90.00   38
  4  \w    135.00 176.00   1.00    1.00    --   87.33 104.00 -90.00   41
  5  \w    140.00 166.00   1.00    1.00    --   87.33 155.00 -43.00   26
  6  \w    134.00 168.00   1.00    1.00    --   87.33 104.00-150.00   34
  7  \w    141.00 174.00   1.00    1.00    --  131.00  77.00 -90.00   33
  8  \w    148.00 174.00   1.00    1.00    --  131.00  77.00-180.00   26
  9  \w    120.00 146.00   1.00    1.00    --  131.00  99.00-180.00   26
 10  \w    106.00 161.00   1.00    1.00    --  131.00  77.00-150.00   55
 11  \w    102.00 177.00   1.00    1.00    --   87.33 104.00 -30.00   75
 12  \w    140.00 175.00   1.00    1.00    --  131.00  43.00  60.00   35
 13  \w    152.00 177.00   1.00    1.00    --  131.00  77.00  30.00   25
 14  \w    138.00 164.00   1.00    1.00    --   98.00  51.00  90.23   26
 15  \w    139.00 165.00   1.00    1.00    --  131.00  65.00 150.00   26
 16  \w    113.00 138.00   1.00    1.00    --  131.00 120.00 158.00   25
 17  \w    111.00 149.00   1.00    1.00    --  131.00  99.00 150.00   38
 18  \w    127.00 165.00   1.00    1.00    --   87.33 138.00  60.00   38
 19  \w    125.00 177.00   1.00    1.00    --  131.00  77.00 -30.00   52
 20  \w    115.00 167.00   1.00    1.00    --  131.00 125.00  60.00   52
 21  \w    107.00 162.00   1.00    1.00    --  131.00  77.00 120.00   55
 22  \w     93.00 123.00   1.00    1.00    --   87.33 138.00  60.00   30
 23  \w     94.00 149.00   1.00    1.00    --   43.67 125.00  60.00   55
 24  \w     88.00 113.00   1.00    1.00    --   43.67 155.00 -43.00   25
 25  \w     74.00 173.00   1.00    1.00    --   87.33  77.00  30.00   99
 26  \w    112.00 138.00   1.00    1.00    --  131.00 178.00-120.00   26
 27  \w     87.00 138.00   1.00    1.00    --  131.00 178.00 -90.00   51
 28  \w     78.00 128.00   1.00    1.00    --  131.00 155.00 -43.00   50
 29  \w     78.00 104.00   1.00    1.00    --  131.00  77.00 -30.00   26
 30  \w     78.00 121.00   1.00    1.00    --  131.00  65.00 -60.00   43
 31  \w     81.00 178.00   1.00    1.00    --  131.00  65.00   0.00   97
 32  \w     81.00 123.00   1.00    1.00    --  131.00  65.00  60.00   42
 33  \w     76.00 140.00   1.00    1.00    --  131.00  77.00  60.00   64
 34  \w     76.00 127.00   1.00    1.00    --  131.00  65.00 -30.00   51
 35  \w     78.00 139.00   1.00    1.00    --  131.00  65.00-120.00   61
 36  \w     81.00 121.00   1.00    1.00    --  131.00  77.00-180.00   40
 37  \w     77.00 127.00   1.00    1.00    --  131.00  65.00-180.00   50
 38  \w     78.00 139.00   1.00    1.00    --  131.00  77.00 -90.00   61
 39  \w     77.00 115.00   1.00    1.00    --  131.00  65.00-150.00   38
 40  \w     77.00 102.00   1.00    1.00    --  131.00  77.00-150.00   25
 41  \w     78.00 147.00   1.00    1.00    --  131.00  77.00-120.00   69
 42  \w     76.00 119.00   1.00    1.00    --  131.00  65.00 -90.00   43
 43  \w     77.00 132.00   1.00    1.00    --  131.00  77.00 -60.00   55
 44  \w     76.00 146.00   1.00    1.00    --  131.00  77.00  30.00   70
 45  \w     77.00 118.00   1.00    1.00    --  131.00  65.00  90.00   41
 46  \w     78.00 132.00   1.00    1.00    --  131.00  65.00 120.00   54
 47  \w     76.00 178.00   1.00    1.00    --  131.00  77.00  90.00  102
 48  \w     76.00 132.00   1.00    1.00    --  131.00  77.00 150.00   56
 49  \w     76.00 102.00   1.00    1.00    --  131.00  77.00 120.00   26
 50  \w     76.00 115.00   1.00    1.00    --  131.00  65.00 150.00   39
 51  \w     69.00  97.00   1.00    1.00    --  131.00  43.00  60.00   28
 52  \w     43.00  71.00   1.00    1.00    --   98.00  77.00 -23.02   28
 53  \w     32.00  58.00   1.00    1.00    --   87.33  77.00  60.00   26
 54  \w     40.00 123.00   1.00    1.00    --   98.00  51.00  90.23   83
 55  \w     38.00  79.00   1.00    1.00    --   98.00  49.00 138.44   41
 56  \w     33.00  69.00   1.00    1.00    --   87.33  77.00  30.00   36
 57  \w     15.00  43.00   1.00    1.00    --   70.00  82.00  96.58   28
 58  \w      5.00  32.00   1.00    1.00    --   62.00  90.00 166.81   27
 59  \w     -2.00  23.00   1.00    1.00    --   58.00  96.00  52.92   25
 60  \w      5.00  30.00   1.00    1.00    --   62.00  90.00   9.79   25
 61  \w      6.00  32.00   1.00    1.00    --   62.00  89.00 -10.66   26
 62  \w     -1.00  26.00   1.00    1.00    --   58.00  93.00 -50.81   27
 63  \w     -9.00  16.00   1.00    1.00    --   54.00 104.00-111.96   25
 64  \w     34.00  61.00   1.00    1.00    --   87.33  77.00-150.00   27
 65  \w     35.00  77.00   1.00    1.00    --   94.00  50.00 -66.71   42
 66  \w     23.00 178.00   1.00    1.00    --  131.00 -32.00   0.00  155
 67  \w    107.00 173.00   1.00    1.00    --  131.00 -89.00-120.00   66
 68  \w    122.00 169.00   1.00    1.00    --  131.00 -77.00-150.00   47
 69  \w     88.00 133.00   1.00    1.00    --  131.00-155.00 -82.00   45
 70  \w     77.00 102.00   1.00    1.00    --  131.00 -99.00   0.00   25
 71  \w     58.00 119.00   1.00    1.00    --  131.00-120.00  75.00   61
 72  \w    144.00 178.00   1.00    1.00    --  131.00 -89.00 150.00   34
 73  \w     55.00 104.00   1.00    1.00    --  131.00 -99.00  90.00   49
 74  \w     55.00 156.00   1.00    1.00    --  131.00 -65.00  30.00  101
 75  \w     72.00  97.00   1.00    1.00    --  131.00 -77.00-150.00   25
 76  \w     51.00  88.00   1.00    1.00    --  131.00 -89.00-120.00   37
 77  \w     54.00  96.00   1.00    1.00    --  131.00 -99.00-150.00   42
 78  \w     25.00 107.00   1.00    1.00    --  131.00 -99.00 -90.00   82
 79  \w     34.00  60.00   1.00    1.00    --  131.00 -99.00   0.00   26
 80  \w     28.00  54.00   1.00    1.00    --  131.00-120.00  75.00   26
 81  \w     52.00  78.00   1.00    1.00    --  131.00 -89.00 150.00   26
 82  \w     50.00  83.00   1.00    1.00    --   43.67-120.00  75.00   33
 83  \w     21.00  46.00   1.00    1.00    --    0.00-120.00  75.00   25
 84  \w      7.00  51.00   1.00    1.00    --    0.00 -99.00   0.00   44
 85  \w      2.00  48.00   1.00    1.00    --    0.00 -99.00 -30.00   46
 86  \w     10.00  60.00   1.00    1.00    --    0.00 -99.00-120.00   50
 87  \w    -56.00 -31.00   1.00    1.00    --  -86.50 -77.00  30.00   25
 88  \w    -62.00 -33.00   1.00    1.00    --  -86.50 -77.00 -30.00   29
 89  \w    -61.00 -35.00   1.00    1.00    --  -86.50 -72.00   3.00   26
 90  \w    -59.00 -33.00   1.00    1.00    --  -86.50 -77.00 -60.00   26
 91  \w    -66.00 -33.00   1.00    1.00    --  -86.50 -75.00 -82.75   33
 92  \w    -58.00 -33.00   1.00    1.00    --  -86.50 -77.00-120.00   25
 93  \w    -61.00 -31.00   1.00    1.00    --  -86.50 -77.00-168.90   30
 94  \w    -61.00 -31.00   1.00    1.00    --  -86.50 -77.00-150.00   30
 95  \w    -86.00 -60.00   1.00    1.00    --  -43.67-155.00 -82.00   26
 96  \w   -106.00 -81.00   1.00    1.00    --    0.00-155.00 -82.00   25
 97  \w   -134.00 -80.00   1.00    1.00    --  -43.67 -99.00-150.00   54
 98  \w   -117.00 -75.00   1.00    1.00    --  -86.50 -77.00-150.00   42
 99  \w    -92.00 -67.00   1.00    1.00    --  -86.50 -77.00-168.90   25
100  \w   -129.00 -81.00   1.00    1.00    --  -86.50-104.00-150.00   48
101  \w   -145.00-110.00   1.00    1.00    --  -86.50-155.00 -82.00   35
102  \w   -152.00-102.00   1.00    1.00    --  -43.67 -99.00 -60.00   50
103  \w   -109.00   0.00   1.00    1.00    --  -43.67 -57.00   0.00  109
104  \w    -63.00 -21.00   1.00    1.00    --  -43.67 -57.00  90.00   42
105  \w    -65.00 -35.00   1.00    1.00    --  -86.50 -77.00  73.63   30
106  \w    -64.00 -31.00   1.00    1.00    --  -86.50 -77.00  98.92   33
107  \w    -79.00  50.00   1.00    1.00    --  -43.67 -19.00 120.00  129
108  \w    -53.00 -28.00   1.00    1.00    --  -86.50 120.00 158.00   25
109  \w    -48.00 -18.00   1.00    1.00    --    0.00 120.00 158.00   30
110  \w    -30.00  -5.00   1.00    1.00    --   43.67 123.00-174.66   25
111  \w    -89.00 -64.00   1.00    1.00    --  -86.50 155.00 -43.00   25
112  \w   -142.00 -83.00   1.00    1.00    --  -43.67 -19.00 120.00   59
113  \w   -125.00 -88.00   1.00    1.00    --  -43.67 -57.00  90.00   37
114  \w   -134.00 -87.00   1.00    1.00    --  -43.67 -99.00  90.00   47
115  \w    -99.00 -33.00   1.00    1.00    --  -86.50 -73.00 123.91   66
116  \w   -142.00-106.00   1.00    1.00    --  -86.50 -77.00  73.63   36
117  \w   -149.00 -82.00   1.00    1.00    --  -43.67-120.00  75.00   67
118  \w   -146.00 -73.00   1.00    1.00    --  -86.50 -77.00 -30.00   73
119  \w   -151.00-126.00   1.00    1.00    --  -86.50-120.00  75.00   25
120  \w   -154.00 -76.00   1.00    1.00    --  -86.50 -77.00  30.00   78
121  \w   -146.00 -97.00   1.00    1.00    --  -86.50 -75.00 -82.75   49
122  \w   -160.00-135.00   1.00    1.00    --  -86.50-104.00-150.00   25
123  \w   -167.00-141.00   1.00    1.00    --  -86.50 -77.00-150.00   26
124  \w   -177.00 -74.00   1.00    1.00    --  -86.50 -77.00-120.00  103
125  \w   -177.00 -77.00   1.00    1.00    --  -86.50 -77.00 -60.00  100
126  \w   -176.00-122.00   1.00    1.00    --  -86.50 -73.00 123.91   54
127  \w   -140.00 -41.00   1.00    1.00    --  -86.50 -64.00 150.00   99
128  \w   -176.00 -75.00   1.00    1.00    --  -86.50 -72.00   3.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0360690000
_diffrn_orient_matrix_UB_12      0.1929783000
_diffrn_orient_matrix_UB_13      -0.0569584000
_diffrn_orient_matrix_UB_21      -0.0721911000
_diffrn_orient_matrix_UB_22      0.1041303000
_diffrn_orient_matrix_UB_23      -0.0337180000
_diffrn_orient_matrix_UB_31      0.0091810000
_diffrn_orient_matrix_UB_32      0.0603530000
_diffrn_orient_matrix_UB_33      0.2402638000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1652
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5708
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.450
_diffrn_reflns_theta_min         4.664
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.306
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.791
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.313
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         891
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1669P)^2^+3.1476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                860
_reflns_number_total             891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119865.cif
_cod_data_source_block           exp_3224_twin1_hklf4
_cod_depositor_comments
;

2022-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         204.61
_cod_original_formula_moiety         '0.5(C10 H14 Mn N4 O8), H2 O'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C5 H9 Mn0.50 N2 O5'
_cod_database_code               1564076
_chemical_oxdiff_formula         'C20  H36  Mn2  N8  O20  '
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.193
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained planarity
 C5, C4, C7, O2, H2WA, O2W, H2WB
 with sigma of 0.1
3.a Free rotating group:
 O2W(H2WA,H2WB)
3.b Rotating group:
 O1W(H1WA,H1WB)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
;