#------------------------------------------------------------------------------
#$Date: 2020-10-21 08:08:37 +0300 (Wed, 21 Oct 2020) $
#$Revision: 258513 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/36/2243633.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243633
loop_
_publ_author_name
'Sarr, Mamour'
'Diop, Mayoro'
'Thiam, Elhadj Ibrahima'
'Barry, Aliou Hamady'
'Gaye, Mohamed'
'Retailleau, Pascal'
_publ_section_title
;
 Crystal structure of
 aquachlorido(nitrato-κ²O,O')[1-(pyridin-2-yl-κN)-2-(pyridin-2-ylmethylidene-κN)hydrazine-κN²]manganase(II)
;
_journal_coeditor_code           EB2005
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              450
_journal_page_last               453
_journal_paper_doi               10.1107/S2056989018003493
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Mn Cl (N O3) (C11 H10 N4) (H2 O)]'
_chemical_formula_moiety         'C11 H12 Cl Mn N5 O4'
_chemical_formula_sum            'C11 H12 Cl Mn N5 O4'
_chemical_formula_weight         368.65
_chemical_name_systematic
Aquachlorido(nitrato-κ²O,O')[1-(pyridin-2-yl-κN)-2-(pyridin-2-ylmethylidene-κN)hydrazine-κN²]manganase(II)
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                98.784(2)
_cell_angle_beta                 97.636(2)
_cell_angle_gamma                108.308(2)
_cell_formula_units_Z            2
_cell_length_a                   6.96980(10)
_cell_length_b                   10.6055(2)
_cell_length_c                   10.8476(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6423
_cell_measurement_theta_min      2.4120
_cell_volume                     738.21(3)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22026
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.106
_diffrn_reflns_theta_min         3.572
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.464
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0337
_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/[σ²(Fo²)+(0.0431P)²+0.1976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                2905
_reflns_number_total             3571
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            eb2005sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        738.21(2)
_cod_database_code               2243633
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.71914(4) 0.39182(3) 0.74637(2) 0.04153(11) Uani d 1 . .
Cl Cl1 0.33417(8) 0.30415(5) 0.69679(5) 0.05511(14) Uani d 1 . .
O O1W 1.0615(2) 0.46771(14) 0.79278(13) 0.0541(3) Uani d 1 . .
H H1WA 1.140892 0.416765 0.774402 0.081 Uiso d 1 . .
H H1WB 1.118139 0.516748 0.869134 0.081 Uiso d 1 . .
O O2 0.7483(2) 0.38248(13) 0.96166(13) 0.0529(3) Uani d 1 . .
O O3 0.7175(3) 0.19991(15) 0.83256(13) 0.0631(4) Uani d 1 . .
O O4 0.7546(3) 0.20477(18) 1.03568(15) 0.0728(5) Uani d 1 . .
N N1 0.7321(3) 0.61349(16) 0.81806(18) 0.0528(4) Uani d 1 . .
N N2 0.7448(2) 0.50621(19) 0.58471(17) 0.0519(4) Uani d 1 . .
N N3 0.7437(8) 0.4569(8) 0.4755(5) 0.0484(13) Uani d 0.53(2) A 1
H H3N 0.742706 0.499635 0.414304 0.058 Uiso calc 0.53(2) A 1
N N4 0.7511(3) 0.25742(19) 0.56463(15) 0.0550(4) Uani d 1 . .
N N5 0.7400(3) 0.25956(16) 0.94508(15) 0.0474(4) Uani d 1 . .
C C1 0.7239(4) 0.6682(2) 0.9358(2) 0.0651(6) Uani d 1 . .
H H1 0.706417 0.613021 0.995278 0.078 Uiso calc 1 . .
C C2 0.7400(4) 0.8019(2) 0.9744(3) 0.0810(8) Uani d 1 . .
H H2 0.735126 0.835887 1.057767 0.097 Uiso calc 1 . .
C C3 0.7630(5) 0.8828(3) 0.8875(4) 0.0962(11) Uani d 1 . .
H H3 0.773464 0.973219 0.910758 0.115 Uiso calc 1 . .
C C4 0.7707(4) 0.8300(3) 0.7648(4) 0.0840(9) Uani d 1 . .
H H4 0.787019 0.884113 0.704332 0.101 Uiso calc 1 . .
C C5 0.7536(3) 0.6938(2) 0.7329(3) 0.0593(6) Uani d 1 . .
C C6 0.757(2) 0.6350(13) 0.6090(13) 0.072(6) Uani d 0.53(2) A 1
H H6 0.766705 0.684993 0.545312 0.087 Uiso calc 0.53(2) A 1
C C7 0.7444(3) 0.3077(3) 0.45798(19) 0.0605(6) Uani d 1 . .
C C8 0.7378(4) 0.2313(4) 0.3399(2) 0.0898(10) Uani d 1 . .
H H8 0.732275 0.267981 0.267437 0.108 Uiso calc 1 . .
C C9 0.7394(5) 0.1032(4) 0.3320(3) 0.1050(13) Uani d 1 . .
H H9 0.732556 0.050255 0.253735 0.126 Uiso calc 1 . .
C C10 0.7511(5) 0.0521(3) 0.4395(3) 0.0934(10) Uani d 1 . .
H H10 0.754750 -0.035280 0.435722 0.112 Uiso calc 1 . .
C C11 0.7575(4) 0.1323(3) 0.5545(2) 0.0744(7) Uani d 1 . .
H H11 0.766778 0.097228 0.627718 0.089 Uiso calc 1 . .
C C6A 0.7462(14) 0.4203(12) 0.4658(9) 0.051(2) Uiso d 0.47(2) A 2
H H6A 0.748686 0.456233 0.392738 0.061 Uiso calc 0.47(2) A 2
N N3A 0.755(2) 0.6312(11) 0.6045(10) 0.057(4) Uiso d 0.47(2) A 2
H H3NA 0.761514 0.675558 0.544192 0.069 Uiso calc 0.47(2) A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1W Mn1 N2 . . 87.38(6) ?
O1W Mn1 N4 . . 85.96(6) ?
N2 Mn1 N4 . . 69.62(7) ?
O1W Mn1 N1 . . 87.94(5) ?
N2 Mn1 N1 . . 69.85(7) ?
N4 Mn1 N1 . . 139.23(7) ?
O1W Mn1 O2 . . 83.70(5) ?
N2 Mn1 O2 . . 152.55(6) ?
N4 Mn1 O2 . . 135.11(6) ?
N1 Mn1 O2 . . 83.90(6) ?
O1W Mn1 O3 . . 89.13(6) ?
N2 Mn1 O3 . . 151.72(6) ?
N4 Mn1 O3 . . 82.14(6) ?
N1 Mn1 O3 . . 138.06(6) ?
O2 Mn1 O3 . . 54.21(5) ?
O1W Mn1 Cl1 . . 179.07(4) ?
N2 Mn1 Cl1 . . 93.54(4) ?
N4 Mn1 Cl1 . . 94.25(5) ?
N1 Mn1 Cl1 . . 92.48(4) ?
O2 Mn1 Cl1 . . 95.52(4) ?
O3 Mn1 Cl1 . . 90.00(5) ?
Mn1 O1W H1WA . . 124.5 ?
Mn1 O1W H1WB . . 116.1 ?
H1WA O1W H1WB . . 105.9 ?
N5 O2 Mn1 . . 95.09(10) ?
N5 O3 Mn1 . . 94.39(10) ?
C1 N1 C5 . . 117.34(19) ?
C1 N1 Mn1 . . 126.26(14) ?
C5 N1 Mn1 . . 116.38(16) ?
N3 N2 C6 . . 116.9(6) ?
N3A N2 C6A . . 128.2(6) ?
N3 N2 Mn1 . . 124.8(4) ?
N3A N2 Mn1 . . 120.1(5) ?
C6 N2 Mn1 . . 118.4(6) ?
C6A N2 Mn1 . . 111.7(5) ?
N2 N3 C7 . . 113.2(4) ?
N2 N3 H3N . . 123.4 ?
C7 N3 H3N . . 123.4 ?
C11 N4 C7 . . 117.6(2) ?
C11 N4 Mn1 . . 126.03(15) ?
C7 N4 Mn1 . . 116.15(16) ?
O4 N5 O3 . . 122.94(16) ?
O4 N5 O2 . . 120.77(16) ?
O3 N5 O2 . . 116.29(15) ?
N1 C1 C2 . . 123.8(3) ?
N1 C1 H1 . . 118.1 ?
C2 C1 H1 . . 118.1 ?
C3 C2 C1 . . 118.4(3) ?
C3 C2 H2 . . 120.8 ?
C1 C2 H2 . . 120.8 ?
C2 C3 C4 . . 119.6(2) ?
C2 C3 H3 . . 120.2 ?
C4 C3 H3 . . 120.2 ?
C3 C4 C5 . . 118.7(3) ?
C3 C4 H4 . . 120.6 ?
C5 C4 H4 . . 120.6 ?
N1 C5 C4 . . 122.1(3) ?
N1 C5 C6 . . 117.1(4) ?
C4 C5 C6 . . 120.8(5) ?
N1 C5 N3A . . 116.5(5) ?
C4 C5 N3A . . 121.4(5) ?
N2 C6 C5 . . 118.3(7) ?
N2 C6 H6 . . 120.9 ?
C5 C6 H6 . . 120.9 ?
C6A C7 N4 . . 118.6(5) ?
C6A C7 C8 . . 119.5(5) ?
N4 C7 C8 . . 122.0(3) ?
N4 C7 N3 . . 115.6(2) ?
C8 C7 N3 . . 122.4(3) ?
C9 C8 C7 . . 119.1(3) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 119.5(3) ?
C8 C9 H9 . . 120.2 ?
C10 C9 H9 . . 120.2 ?
C9 C10 C11 . . 119.0(3) ?
C9 C10 H10 . . 120.5 ?
C11 C10 H10 . . 120.5 ?
N4 C11 C10 . . 122.7(3) ?
N4 C11 H11 . . 118.6 ?
C10 C11 H11 . . 118.6 ?
C7 C6A N2 . . 123.3(8) ?
C7 C6A H6A . . 118.4 ?
N2 C6A H6A . . 118.4 ?
N2 N3A C5 . . 117.1(8) ?
N2 N3A H3NA . . 121.5 ?
C5 N3A H3NA . . 121.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1W . 2.2239(14) y
Mn1 N2 . 2.2750(16) y
Mn1 N4 . 2.3292(16) y
Mn1 N1 . 2.3300(16) y
Mn1 O2 . 2.3372(14) y
Mn1 O3 . 2.3635(15) y
Mn1 Cl1 . 2.4999(6) y
O1W H1WA . 0.9067 ?
O1W H1WB . 0.8745 ?
O2 N5 . 1.270(2) ?
O3 N5 . 1.251(2) ?
O4 N5 . 1.224(2) ?
N1 C1 . 1.337(3) ?
N1 C5 . 1.341(3) ?
N2 N3 . 1.217(7) y
N2 N3A . 1.288(11) y
N2 C6 . 1.325(13) y
N2 C6A . 1.465(10) y
N3 C7 . 1.566(9) y
N3 H3N . 0.8600 ?
N4 C11 . 1.330(3) ?
N4 C7 . 1.347(3) ?
C1 C2 . 1.380(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.361(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.378(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.396(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.398(15) y
C5 N3A . 1.450(11) y
C6 H6 . 0.9300 ?
C7 C6A . 1.180(11) y
C7 C8 . 1.394(3) ?
C8 C9 . 1.352(5) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.362(5) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.386(3) ?
C10 H10 . 0.9300 ?
C11 H11 . 0.9300 ?
C6A H6A . 0.9300 ?
N3A H3NA . 0.8600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1WA Cl1 1_655 0.91 2.23 3.1225(15) 169.8
O1W H1WB O2 2_767 0.87 1.92 2.7969(19) 176.6
O1W H1WB N5 2_767 0.87 2.68 3.506(2) 157.1
N3 H3N Cl1 2_666 0.86 2.71 3.501(7) 152.7
C1 H1 O2 . 0.93 2.53 3.140(3) 123.5
C6 H6 Cl1 2_666 0.93 2.66 3.489(11) 149.4
C8 H8 O4 1_554 0.93 2.54 3.290(3) 138.0
C10 H10 Cl1 2_656 0.93 2.83 3.669(3) 151.5
C11 H11 O3 . 0.93 2.44 3.062(3) 124.6

_cod_database_fobs_code 2243633
