#------------------------------------------------------------------------------
#$Date: 2020-05-23 08:16:07 +0300 (Sat, 23 May 2020) $
#$Revision: 252320 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/34/2243406.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_2243406
loop_
_publ_author_name
'Khosa, Muhammad Kaleem'
'Wood, Paul T.'
'Humphrey, Simon M.'
'Harrison, William T. A.'
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of
 poly[bis(μ₃-3,4-diaminobenzoato)manganese], a layered coordination
 polymer
;
_journal_coeditor_code           IS5538
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              909
_journal_page_last               913
_journal_paper_doi               10.1107/S2056989020006805
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Mn (C7 H7 N2 O2)2]'
_chemical_formula_moiety         'C14 H14 Mn N4 O4'
_chemical_formula_sum            'C14 H14 Mn N4 O4'
_chemical_formula_weight         357.23
_chemical_name_systematic
Poly[bis(μ₃-3,4-diaminobenzoato-κ³N³,O,O')manganese(II)]
_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
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 104.698(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5171(5)
_cell_length_b                   4.4212(2)
_cell_length_c                   13.9752(7)
_cell_measurement_reflns_used    5315
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.02
_cell_volume                     688.32(6)
_computing_cell_refinement
;
HKL Scalepack (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997),
SORTAV (Blessing, 1995)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Shape Software,
2007)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5289
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         2.053
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       slab
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.275
_refine_ls_extinction_coef       0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0310
_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/[σ²(Fo²)+(0.0282P)²+0.5090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                1105
_reflns_number_total             1345
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            is5538sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243406
_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.
;
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.952
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.000000 0.500000 0.000000 0.01883(17) Uani d 1 . .
C C1 0.32186(18) -0.0488(5) 0.11717(15) 0.0195(5) Uani d 1 . .
C C2 0.36414(18) 0.1055(5) 0.20598(15) 0.0198(5) Uani d 1 . .
H H2 0.312438 0.241153 0.228031 0.024 Uiso calc 1 . .
C C3 0.48037(18) 0.0642(5) 0.26264(15) 0.0192(5) Uani d 1 . .
C C4 0.55799(18) -0.1335(5) 0.23063(16) 0.0204(5) Uani d 1 . .
C C5 0.51634(19) -0.2802(5) 0.13985(17) 0.0254(5) Uani d 1 . .
H H5 0.568982 -0.407707 0.115733 0.030 Uiso calc 1 . .
C C6 0.39925(19) -0.2419(5) 0.08470(16) 0.0242(5) Uani d 1 . .
H H6 0.371484 -0.348284 0.024144 0.029 Uiso calc 1 . .
C C7 0.19402(18) -0.0122(5) 0.06079(14) 0.0181(4) Uani d 1 . .
N N1 0.52161(17) 0.2169(4) 0.35541(13) 0.0205(4) Uani d 1 . .
H H1N 0.482(2) 0.387(6) 0.3585(18) 0.025 Uiso d 1 . .
H H2N 0.596(2) 0.262(6) 0.3646(18) 0.025 Uiso d 1 . .
N N2 0.67763(16) -0.1663(5) 0.28747(15) 0.0229(4) Uani d 1 . .
H H3N 0.716(2) -0.306(6) 0.2669(18) 0.028 Uiso d 1 . .
H H4N 0.681(2) -0.190(6) 0.350(2) 0.028 Uiso d 1 . .
O O1 0.13370(12) 0.1975(3) 0.08586(11) 0.0224(4) Uani d 1 . .
O O2 0.15011(13) -0.1998(3) -0.00841(11) 0.0229(4) Uani d 1 . .
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'
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
O1 Mn1 O1 . 3_565 180.0 ?
O1 Mn1 O2 . 3 93.20(6) ?
O1 Mn1 O2 3_565 3 86.80(6) ?
O1 Mn1 O2 . 1_565 86.80(6) ?
O1 Mn1 O2 3_565 1_565 93.20(6) ?
O2 Mn1 O2 3 1_565 180.0 ?
O1 Mn1 N1 . 4_565 90.52(6) ?
O1 Mn1 N1 3_565 4_565 89.48(6) ?
O2 Mn1 N1 3 4_565 93.25(6) ?
O2 Mn1 N1 1_565 4_565 86.75(6) ?
O1 Mn1 N1 . 2 89.48(6) ?
O1 Mn1 N1 3_565 2 90.52(6) ?
O2 Mn1 N1 3 2 86.75(6) ?
O2 Mn1 N1 1_565 2 93.25(6) ?
N1 Mn1 N1 4_565 2 180.0 ?
C6 C1 C2 . . 118.93(19) ?
C6 C1 C7 . . 121.50(18) ?
C2 C1 C7 . . 119.54(19) ?
C3 C2 C1 . . 121.0(2) ?
C3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C2 C3 C4 . . 120.14(19) ?
C2 C3 N1 . . 120.44(19) ?
C4 C3 N1 . . 119.41(18) ?
C5 C4 C3 . . 118.65(19) ?
C5 C4 N2 . . 121.6(2) ?
C3 C4 N2 . . 119.64(19) ?
C6 C5 C4 . . 120.7(2) ?
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C5 C6 C1 . . 120.6(2) ?
C5 C6 H6 . . 119.7 ?
C1 C6 H6 . . 119.7 ?
O1 C7 O2 . . 123.23(18) ?
O1 C7 C1 . . 118.20(18) ?
O2 C7 C1 . . 118.53(19) ?
C3 N1 Mn1 . 2_545 120.83(14) ?
C3 N1 H1N . . 112.9(16) ?
Mn1 N1 H1N 2_545 . 98.0(16) ?
C3 N1 H2N . . 109.6(17) ?
Mn1 N1 H2N 2_545 . 107.0(17) ?
H1N N1 H2N . . 107(2) ?
C4 N2 H3N . . 113.5(17) ?
C4 N2 H4N . . 111.1(16) ?
H3N N2 H4N . . 111(2) ?
C7 O1 Mn1 . . 131.83(13) ?
C7 O2 Mn1 . 1_545 121.03(13) ?
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 O1 . 2.1591(14) ?
Mn1 O1 3_565 2.1591(14) ?
Mn1 O2 3 2.2062(15) ?
Mn1 O2 1_565 2.2062(15) ?
Mn1 N1 4_565 2.3065(19) ?
Mn1 N1 2 2.3065(19) ?
C1 C6 . 1.391(3) ?
C1 C2 . 1.392(3) ?
C1 C7 . 1.492(3) ?
C2 C3 . 1.384(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.402(3) ?
C3 N1 . 1.432(3) ?
C4 C5 . 1.397(3) ?
C4 N2 . 1.413(3) ?
C5 C6 . 1.383(3) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 O1 . 1.261(3) ?
C7 O2 . 1.277(3) ?
N1 H1N . 0.88(3) ?
N1 H2N . 0.86(3) ?
N2 H3N . 0.85(3) ?
N2 H4N . 0.88(3) ?
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
_geom_hbond_publ_flag
N1 H1N O1 2 0.88(3) 2.19(3) 3.022(3) 156(2) yes
N2 H3N N2 2_645 0.85(3) 2.26(3) 3.106(3) 178(2) yes
N2 H4N O2 4_656 0.88(3) 2.15(3) 3.008(2) 167(2) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -1.4(3) ?
C7 C1 C2 C3 . . . . 176.57(19) ?
C1 C2 C3 C4 . . . . 0.5(3) ?
C1 C2 C3 N1 . . . . -178.0(2) ?
C2 C3 C4 C5 . . . . 1.6(3) ?
N1 C3 C4 C5 . . . . -179.9(2) ?
C2 C3 C4 N2 . . . . 177.9(2) ?
N1 C3 C4 N2 . . . . -3.5(3) ?
C3 C4 C5 C6 . . . . -2.9(3) ?
N2 C4 C5 C6 . . . . -179.1(2) ?
C4 C5 C6 C1 . . . . 2.0(3) ?
C2 C1 C6 C5 . . . . 0.1(3) ?
C7 C1 C6 C5 . . . . -177.8(2) ?
C6 C1 C7 O1 . . . . -169.7(2) ?
C2 C1 C7 O1 . . . . 12.4(3) ?
C6 C1 C7 O2 . . . . 12.3(3) ?
C2 C1 C7 O2 . . . . -165.55(19) ?
C2 C3 N1 Mn1 . . . 2_545 89.4(2) ?
C4 C3 N1 Mn1 . . . 2_545 -89.1(2) ?
O2 C7 O1 Mn1 . . . . -40.5(3) ?
C1 C7 O1 Mn1 . . . . 141.59(15) ?
O1 C7 O2 Mn1 . . . 1_545 -60.8(2) ?
C1 C7 O2 Mn1 . . . 1_545 117.02(17) ?

_cod_database_fobs_code 2243406
