#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/08/7050869.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_7050869
loop_
_publ_author_name
'Dalai, Sudipta'
'Sarathi Mukherjee, Partha'
'Zangrando, Ennio'
'Ray Chaudhuri, Nirmalendu'
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of two new
 dicyanamide bridged 2D and 1D complexes of Mn(ii)
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1185
_journal_paper_doi               10.1039/b202431b
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         '2(C6 H4 N2) 2(N3 C2 1-) (Mn 2+)'
_chemical_formula_sum            'C16 H8 Mn N10'
_chemical_formula_weight         395.26
_chemical_name_systematic
;
bis(4-cyanopyridine)-bis(dicyanamide)-manganese(II)
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.479(4)
_cell_length_b                   12.308(5)
_cell_length_c                   14.402(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1680.2(11)
_computing_cell_refinement       'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_data_collection       'Nonius Xpress'
_computing_data_reduction        'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.64.02 (Farrugia, 1999)'
_computing_structure_refinement  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4276
_diffrn_reflns_theta_full        28.81
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            'no colour'
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0692P)²+0.2108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                1801
_reflns_number_total             2179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202431b.txt
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7050869
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.7500 -0.2500 -0.14980(2) 0.03990(16) Uani 1 2 d S . .
N1 N 0.60343(15) -0.16964(11) -0.03808(10) 0.0459(3) Uani 1 1 d . . .
C1 C 0.65825(18) -0.13273(14) 0.04155(12) 0.0479(4) Uani 1 1 d . . .
H1 H 0.7555 -0.1234 0.0449 0.057 Uiso 1 1 calc R . .
C2 C 0.57885(19) -0.10770(16) 0.11895(14) 0.0496(4) Uani 1 1 d . . .
H2 H 0.6214 -0.0839 0.1734 0.059 Uiso 1 1 calc R . .
C3 C 0.43387(19) -0.11914(14) 0.11299(13) 0.0467(4) Uani 1 1 d . . .
C4 C 0.37440(19) -0.14809(16) 0.02878(14) 0.0548(4) Uani 1 1 d . . .
H4 H 0.2770 -0.1499 0.0214 0.066 Uiso 1 1 calc R . .
C5 C 0.4628(2) -0.17428(16) -0.04415(14) 0.0545(4) Uani 1 1 d . . .
H5 H 0.4226 -0.1962 -0.1000 0.065 Uiso 1 1 calc R . .
N2 N 0.2805(2) -0.10118(18) 0.26095(15) 0.0715(5) Uani 1 1 d . . .
C6 C 0.34739(19) -0.10659(16) 0.19539(15) 0.0554(4) Uani 1 1 d . . .
N3 N 0.49771(19) -0.07373(14) -0.38039(11) 0.0569(4) Uani 1 1 d . . .
N4 N 0.61221(17) -0.17464(12) -0.25485(10) 0.0510(4) Uani 1 1 d . . .
N5 N 0.88266(17) -0.10458(13) -0.13112(12) 0.0519(4) Uani 1 1 d . . .
C7 C 0.55625(17) -0.12275(14) -0.31052(12) 0.0442(4) Uani 1 1 d . . .
C8 C 0.93898(18) -0.02153(14) -0.12947(12) 0.0449(4) Uani 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 0.0033 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Mn N4 93.28(8) . 2_645 ?
N4 Mn N5 95.02(6) . 2_645 ?
N4 Mn N5 94.60(6) 2_645 2_645 ?
N4 Mn N5 94.60(6) . . ?
N4 Mn N5 95.02(6) 2_645 . ?
N5 Mn N5 165.97(9) 2_645 . ?
N4 Mn N1 179.94(6) . 2_645 ?
N4 Mn N1 86.69(6) 2_645 2_645 ?
N5 Mn N1 84.94(6) 2_645 2_645 ?
N5 Mn N1 85.45(6) . 2_645 ?
N4 Mn N1 86.69(6) . . ?
N4 Mn N1 179.94(6) 2_645 . ?
N5 Mn N1 85.45(6) 2_645 . ?
N5 Mn N1 84.94(6) . . ?
N1 Mn N1 93.33(8) 2_645 . ?
C5 N1 C1 117.23(15) . . ?
C5 N1 Mn 121.86(12) . . ?
C1 N1 Mn 120.07(11) . . ?
N1 C1 C2 123.79(16) . . ?
C1 C2 C3 117.95(17) . . ?
C4 C3 C2 119.01(17) . . ?
C4 C3 C6 120.94(17) . . ?
C2 C3 C6 119.97(17) . . ?
C5 C4 C3 118.64(17) . . ?
N1 C5 C4 123.01(17) . . ?
N2 C6 C3 177.1(2) . . ?
C7 N3 C8 121.03(16) . 3_454 ?
C7 N4 Mn 169.21(15) . . ?
C8 N5 Mn 170.51(16) . . ?
N4 C7 N3 172.90(18) . . ?
N5 C8 N3 174.5(2) . 3_554 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn N4 2.2034(15) . ?
Mn N4 2.2034(15) 2_645 ?
Mn N5 2.2039(16) 2_645 ?
Mn N5 2.2039(16) . ?
Mn N1 2.3447(15) 2_645 ?
Mn N1 2.3447(15) . ?
N1 C5 1.337(2) . ?
N1 C1 1.339(2) . ?
C1 C2 1.380(3) . ?
C2 C3 1.384(3) . ?
C3 C4 1.384(3) . ?
C3 C6 1.451(3) . ?
C4 C5 1.382(3) . ?
N2 C6 1.139(3) . ?
N3 C7 1.298(2) . ?
N3 C8 1.306(2) 3_454 ?
N4 C7 1.154(2) . ?
N5 C8 1.153(2) . ?
C8 N3 1.306(2) 3_554 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Mn N1 C5 46.15(15) . . . . ?
N4 Mn N1 C5 106(100) 2_645 . . . ?
N5 Mn N1 C5 -49.15(15) 2_645 . . . ?
N5 Mn N1 C5 141.07(15) . . . . ?
N1 Mn N1 C5 -133.80(16) 2_645 . . . ?
N4 Mn N1 C1 -144.62(13) . . . . ?
N4 Mn N1 C1 -85(100) 2_645 . . . ?
N5 Mn N1 C1 120.07(13) 2_645 . . . ?
N5 Mn N1 C1 -49.70(13) . . . . ?
N1 Mn N1 C1 35.43(11) 2_645 . . . ?
C5 N1 C1 C2 5.2(3) . . . . ?
Mn N1 C1 C2 -164.51(14) . . . . ?
N1 C1 C2 C3 -1.5(3) . . . . ?
C1 C2 C3 C4 -4.1(3) . . . . ?
C1 C2 C3 C6 172.56(17) . . . . ?
C2 C3 C4 C5 5.9(3) . . . . ?
C6 C3 C4 C5 -170.76(18) . . . . ?
C1 N1 C5 C4 -3.3(3) . . . . ?
Mn N1 C5 C4 166.26(15) . . . . ?
C3 C4 C5 N1 -2.2(3) . . . . ?
C4 C3 C6 N2 92(4) . . . . ?
C2 C3 C6 N2 -85(4) . . . . ?
N4 Mn N4 C7 -81.4(8) 2_645 . . . ?
N5 Mn N4 C7 -176.4(8) 2_645 . . . ?
N5 Mn N4 C7 13.9(8) . . . . ?
N1 Mn N4 C7 -142(100) 2_645 . . . ?
N1 Mn N4 C7 98.5(8) . . . . ?
N4 Mn N5 C8 5.6(10) . . . . ?
N4 Mn N5 C8 99.3(10) 2_645 . . . ?
N5 Mn N5 C8 -127.6(10) 2_645 . . . ?
N1 Mn N5 C8 -174.4(10) 2_645 . . . ?
N1 Mn N5 C8 -80.7(10) . . . . ?
Mn N4 C7 N3 106.7(16) . . . . ?
C8 N3 C7 N4 -177.0(15) 3_454 . . . ?
Mn N5 C8 N3 105(2) . . . 3_554 ?
