#------------------------------------------------------------------------------
#$Date: 2021-07-09 11:17:25 +0300 (Fri, 09 Jul 2021) $
#$Revision: 267421 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/40/1564075.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1564075
loop_
_publ_author_name
'Świderski, Grzegorz'
'Łyszczek, Renata'
'Wojtulewski, Sławomir'
'Kalinowska, Monika'
'Świsłocka, Renata'
'Lewandowski, Włodzimierz'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  33.00   1.00    1.00    --  -41.69  66.00 -58.00  106
  2  ω   -117.00 -10.00   1.00    1.00    --  -41.69 -66.00 167.00  107
  3  ω     82.00 178.00   1.00    1.00    --  113.00  66.00 -58.00   96
  4  ω     38.00 144.00   1.00    1.00    --  113.00 -66.00 167.00  106
  5  ω   -124.00 -79.00   1.00    1.00    --  -41.69 -99.00-150.00   45
  6  ω   -124.00 -79.00   1.00    1.00    --  -41.69 -99.00 -90.00   45
  7  ω   -124.00 -79.00   1.00    1.00    --  -41.69 -99.00 -60.00   45
  8  ω     23.00  99.00   1.00    1.00    --   41.69-125.00-180.00   76
  9  ω     23.00  99.00   1.00    1.00    --   41.69-125.00  90.00   76
 10  ω     10.00 117.00   1.00    1.00    --   41.69  66.00 -58.00  107
 11  ω     23.00  99.00   1.00    1.00    --   41.69-125.00 -60.00   76
 12  ω     35.00 116.00   1.00    1.00    --  113.00-111.00 -60.00   81
 13  ω     82.00 178.00   1.00    1.00    --  113.00  30.00-120.00   96
 14  ω     57.00 150.00   1.00    1.00    --  113.00 178.00  90.00   93
 15  ω     57.00 150.00   1.00    1.00    --  113.00 178.00-180.00   93
 16  ω     35.00 116.00   1.00    1.00    --  113.00-111.00 -30.00   81
 17  ω     29.00 109.00   1.00    1.00    --  113.00 -95.00 -30.00   80
 18  ω    117.00 155.00   1.00    1.00    --  113.00  61.00-120.00   38
 19  ω    110.00 147.00   1.00    1.00    --  113.00  77.00   0.00   37
 20  ω     60.00  99.00   1.00    1.00    --  113.00 -45.00 -60.00   39
 21  ω    116.00 141.00   1.00    1.00    --  113.00 -45.00 -60.00   25
 22  ω     84.00 110.00   1.00    1.00    --  113.00  61.00-120.00   26
 23  ω     73.00 109.00   1.00    1.00    --  113.00 -95.00-180.00   36
 24  ω     94.00 142.00   1.00    1.00    --  113.00 -61.00 -60.00   48
 25  ω     35.00  69.00   1.00    1.00    --  113.00 -95.00-180.00   34
 26  ω     30.00  64.00   1.00    1.00    --  113.00 -95.00 120.00   34
 27  ω     70.00 108.00   1.00    1.00    --  113.00 -95.00 120.00   38
 28  ω     33.00  78.00   1.00    1.00    --  113.00 -95.00 150.00   45
 29  ω     81.00 115.00   1.00    1.00    --  113.00-111.00  90.00   34
 30  ω     85.00 170.00   1.00    1.00    --  113.00  61.00 -90.00   85
 31  ω     40.00  67.00   1.00    1.00    --  113.00-111.00   0.00   27
 32  ω    110.00 136.00   1.00    1.00    --  113.00 111.00 -60.00   26
 33  ω     91.00 116.00   1.00    1.00    --  113.00-111.00-180.00   25
 34  ω    105.00 131.00   1.00    1.00    --  113.00 178.00 -90.00   26
 35  ω     87.00 129.00   1.00    1.00    --  113.00  45.00-180.00   42
 36  ω    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       'ω 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/[σ²(Fo²)+(0.0731P)²+0.0114P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            ICA-2020-512-119865.cif
_cod_data_source_block           exp_2929
_cod_database_code               1564075
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.000000 1.000000 0.500000 0.02130(16) Uani 1 2 d S T P . .
O1W O 0.1800(3) 1.1930(2) 0.58956(14) 0.0254(3) Uani 1 1 d . . . . .
O2 O -0.2045(3) 0.7848(2) 0.89536(14) 0.0263(3) Uani 1 1 d . . . . .
O1 O -0.2081(3) 0.9659(2) 0.68637(13) 0.0245(3) Uani 1 1 d . . . . .
O2W O -0.7323(3) 1.0280(2) 0.86508(15) 0.0298(3) Uani 1 1 d . . . . .
N2 N 0.2701(3) 0.7426(2) 0.63910(15) 0.0220(3) Uani 1 1 d . . . . .
N1 N 0.5107(3) 0.6392(2) 0.60642(16) 0.0236(3) Uani 1 1 d . . . . .
C7 C -0.1054(4) 0.8251(3) 0.78234(18) 0.0224(4) Uani 1 1 d . . . . .
C6 C 0.6380(4) 0.4777(3) 0.69249(19) 0.0255(4) Uani 1 1 d . . . . .
H6 H 0.808289 0.404716 0.669175 0.031 Uiso 1 1 calc R . . . .
C4 C 0.2910(4) 0.5191(3) 0.84963(19) 0.0257(4) Uani 1 1 d . . . . .
H4 H 0.212413 0.481497 0.933072 0.031 Uiso 1 1 calc R . . . .
C3 C 0.1639(4) 0.6878(3) 0.75690(18) 0.0221(4) Uani 1 1 d . . . . .
C5 C 0.5345(4) 0.4091(3) 0.8158(2) 0.0272(4) Uani 1 1 d . . . . .
H5 H 0.629045 0.290936 0.873928 0.033 Uiso 1 1 calc R . . . .
H1WA H 0.246(6) 1.156(5) 0.674(3) 0.041(8) Uiso 1 1 d . . . . .
H1WB H 0.297(7) 1.222(5) 0.549(4) 0.043(8) Uiso 1 1 d . . . . .
H2WA H -0.760(6) 1.087(5) 0.938(3) 0.037(7) Uiso 1 1 d . . . . .
H2WB H -0.581(9) 0.950(6) 0.871(4) 0.063(11) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 4 3 0.1012
0 -4 -3 0.1012
0 0 -6 0.0608
0 0 6 0.0608
-3 -3 2 0.1811
3 3 3 0.0887
-1 0 -6 0.0807
0 -4 2 0.0937
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1W Mn1 O1W 180.00(6) . 2_576
O1W Mn1 N2 90.27(5) 2_576 .
O1W Mn1 N2 90.27(5) . 2_576
O1W Mn1 N2 89.73(5) . .
O1W Mn1 N2 89.73(5) 2_576 2_576
O1 Mn1 O1W 90.29(5) . 2_576
O1 Mn1 O1W 89.71(5) 2_576 2_576
O1 Mn1 O1W 89.71(5) . .
O1 Mn1 O1W 90.29(5) 2_576 .
O1 Mn1 O1 180.0 . 2_576
O1 Mn1 N2 74.82(5) 2_576 2_576
O1 Mn1 N2 105.18(5) . 2_576
O1 Mn1 N2 105.18(5) 2_576 .
O1 Mn1 N2 74.82(5) . .
N2 Mn1 N2 180.0 2_576 .
Mn1 O1W H1WA 118(2) . .
Mn1 O1W H1WB 117(2) . .
H1WA O1W H1WB 102(3) . .
C7 O1 Mn1 119.03(11) . .
H2WA O2W H2WB 110(3) . .
N1 N2 Mn1 124.86(12) . .
C3 N2 Mn1 113.95(11) . .
C3 N2 N1 121.01(16) . .
C6 N1 N2 118.40(16) . .
O2 C7 O1 126.29(17) . .
O2 C7 C3 116.73(16) . .
O1 C7 C3 116.97(15) . .
N1 C6 H6 118.3 . .
N1 C6 C5 123.44(17) . .
C5 C6 H6 118.3 . .
C3 C4 H4 121.3 . .
C5 C4 H4 121.3 . .
C5 C4 C3 117.41(17) . .
N2 C3 C7 114.79(16) . .
N2 C3 C4 122.24(16) . .
C4 C3 C7 122.97(16) . .
C6 C5 H5 121.3 . .
C4 C5 C6 117.45(18) . .
C4 C5 H5 121.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1W 2.2116(14) 2_576
Mn1 O1W 2.2116(14) .
Mn1 O1 2.1387(13) .
Mn1 O1 2.1387(13) 2_576
Mn1 N2 2.2378(16) 2_576
Mn1 N2 2.2378(16) .
O1W H1WA 0.86(3) .
O1W H1WB 0.80(4) .
O2 C7 1.248(2) .
O1 C7 1.260(2) .
O2W H2WA 0.88(3) .
O2W H2WB 0.83(5) .
N2 N1 1.342(2) .
N2 C3 1.331(2) .
N1 C6 1.327(3) .
C7 C3 1.527(2) .
C6 H6 0.9500 .
C6 C5 1.399(3) .
C4 H4 0.9500 .
C4 C3 1.392(3) .
C4 C5 1.373(3) .
C5 H5 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WA O2W 0.86(3) 1.93(3) 2.738(2) 155(3) 1_655 yes
O1W H1WB N1 0.80(4) 2.11(4) 2.873(2) 159(3) 2_676 yes
O2W H2WA O2 0.88(3) 1.99(3) 2.863(2) 176(3) 2_477 yes
O2W H2WB O2 0.83(5) 2.00(5) 2.821(2) 173(4) . yes
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0025 3.9877 2.9969 -0.6344 0.3923 0.5723
0.0025 -3.9877 -2.9969 0.6344 -0.3923 -0.5723
-0.0078 -0.0087 -5.9900 -0.4295 -0.5853 -0.6296
0.0078 0.0087 5.9900 0.4295 0.5853 0.6296
-3.0023 -2.9988 2.0027 0.6096 -0.5113 0.6562
3.0087 3.0061 2.9890 -0.2517 0.9990 -0.1316
-1.0110 -0.0134 -5.9876 -0.4863 -0.7959 -0.4164
0.0089 -3.9804 1.9948 0.9923 0.0955 -0.0476
