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_1564075
_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 H10 Mn N4 O6, 2(H2 O)'
_chemical_formula_sum            'C10 H14 Mn N4 O8'
_chemical_formula_weight         373.19
_chemical_name_systematic
'diaaqua-bis(pyridazine-3-carboxylato)-manganese(II) dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                80.580(5)
_cell_angle_beta                 89.658(6)
_cell_angle_gamma                72.544(6)
_cell_formula_units_Z            1
_cell_length_a                   5.3124(4)
_cell_length_b                   7.3148(4)
_cell_length_c                   9.7421(7)
_cell_measurement_reflns_used    3085
_cell_measurement_temperature    100
_cell_measurement_theta_max      76.0980
_cell_measurement_theta_min      4.5830
_cell_volume                     355.89(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -73.00  33.00   1.00    1.00    --  -41.69  66.00 -58.00  106
  2  \w   -117.00 -10.00   1.00    1.00    --  -41.69 -66.00 167.00  107
  3  \w     82.00 178.00   1.00    1.00    --  113.00  66.00 -58.00   96
  4  \w     38.00 144.00   1.00    1.00    --  113.00 -66.00 167.00  106
  5  \w   -124.00 -79.00   1.00    1.00    --  -41.69 -99.00-150.00   45
  6  \w   -124.00 -79.00   1.00    1.00    --  -41.69 -99.00 -90.00   45
  7  \w   -124.00 -79.00   1.00    1.00    --  -41.69 -99.00 -60.00   45
  8  \w     23.00  99.00   1.00    1.00    --   41.69-125.00-180.00   76
  9  \w     23.00  99.00   1.00    1.00    --   41.69-125.00  90.00   76
 10  \w     10.00 117.00   1.00    1.00    --   41.69  66.00 -58.00  107
 11  \w     23.00  99.00   1.00    1.00    --   41.69-125.00 -60.00   76
 12  \w     35.00 116.00   1.00    1.00    --  113.00-111.00 -60.00   81
 13  \w     82.00 178.00   1.00    1.00    --  113.00  30.00-120.00   96
 14  \w     57.00 150.00   1.00    1.00    --  113.00 178.00  90.00   93
 15  \w     57.00 150.00   1.00    1.00    --  113.00 178.00-180.00   93
 16  \w     35.00 116.00   1.00    1.00    --  113.00-111.00 -30.00   81
 17  \w     29.00 109.00   1.00    1.00    --  113.00 -95.00 -30.00   80
 18  \w    117.00 155.00   1.00    1.00    --  113.00  61.00-120.00   38
 19  \w    110.00 147.00   1.00    1.00    --  113.00  77.00   0.00   37
 20  \w     60.00  99.00   1.00    1.00    --  113.00 -45.00 -60.00   39
 21  \w    116.00 141.00   1.00    1.00    --  113.00 -45.00 -60.00   25
 22  \w     84.00 110.00   1.00    1.00    --  113.00  61.00-120.00   26
 23  \w     73.00 109.00   1.00    1.00    --  113.00 -95.00-180.00   36
 24  \w     94.00 142.00   1.00    1.00    --  113.00 -61.00 -60.00   48
 25  \w     35.00  69.00   1.00    1.00    --  113.00 -95.00-180.00   34
 26  \w     30.00  64.00   1.00    1.00    --  113.00 -95.00 120.00   34
 27  \w     70.00 108.00   1.00    1.00    --  113.00 -95.00 120.00   38
 28  \w     33.00  78.00   1.00    1.00    --  113.00 -95.00 150.00   45
 29  \w     81.00 115.00   1.00    1.00    --  113.00-111.00  90.00   34
 30  \w     85.00 170.00   1.00    1.00    --  113.00  61.00 -90.00   85
 31  \w     40.00  67.00   1.00    1.00    --  113.00-111.00   0.00   27
 32  \w    110.00 136.00   1.00    1.00    --  113.00 111.00 -60.00   26
 33  \w     91.00 116.00   1.00    1.00    --  113.00-111.00-180.00   25
 34  \w    105.00 131.00   1.00    1.00    --  113.00 178.00 -90.00   26
 35  \w     87.00 129.00   1.00    1.00    --  113.00  45.00-180.00   42
 36  \w    108.00 176.00   1.00    1.00    --  113.00 111.00-180.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0578133000
_diffrn_orient_matrix_UB_12      -0.2131162000
_diffrn_orient_matrix_UB_13      0.0719376000
_diffrn_orient_matrix_UB_21      0.2099923000
_diffrn_orient_matrix_UB_22      0.0253068000
_diffrn_orient_matrix_UB_23      0.0974098000
_diffrn_orient_matrix_UB_31      -0.2125243000
_diffrn_orient_matrix_UB_32      0.0642566000
_diffrn_orient_matrix_UB_33      0.1052873000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4325
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.274
_diffrn_reflns_theta_min         4.606
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.045
_exptl_absorpt_correction_T_max  0.298
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       block
_exptl_crystal_F_000             191
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.0114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1470
_reflns_number_total             1486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119865.cif
_cod_data_source_block           exp_2929
_cod_database_code               1564075
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     76.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C5(H5)
;