#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312969.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_4312969
loop_
_publ_author_name
'Albert Escuer'
'Núria Sanz'
'Ramon Vicente'
'Franz A. Mautner'
_publ_section_title
;
 Molecular, 1D, and 2D Systems Built from Phenylcyanamido Ligands.
 Syntheses, Crystal Structures, and Characterization of Their Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              541
_journal_page_last               551
_journal_paper_doi               10.1021/ic025931l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C24 H16 Cl2 Mn N6'
_chemical_formula_weight         514.27
_chemical_name_common            '[Mn(2,2'-bipy)(4-Cl-ph-NCN)2]n'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.45(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.620(4)
_cell_length_b                   10.482(3)
_cell_length_c                   24.860(9)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      4.9
_cell_volume                     2215.7(15)
_computing_molecular_graphics    'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_publication_material  'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'mod. STOE 4-circle diffractometer'
_diffrn_measurement_method       'Omega-scan, delta Omega: 1.30 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2645
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         '3   (-1 2 3; 0 2 0; 2 -1 -3)'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_obs          0.0426
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0485P)²+2.5210P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1256
_refine_ls_wR_factor_obs         0.1043
_reflns_number_observed          1657
_reflns_number_total             1917
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic025931l_s1_4.cif
_cod_data_source_block           ns205b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+2.5210P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+2.5210P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4312969
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn 0.2500 0.64943(5) 0.5000 0.0319(2) Uani 1 d S .
N1 N 0.4910(3) 0.3534(2) 0.47328(10) 0.0406(6) Uani 1 d . .
C1 C 0.3906(3) 0.4226(3) 0.45424(11) 0.0346(6) Uani 1 d . .
N2 N 0.2822(3) 0.5041(2) 0.43595(9) 0.0370(5) Uani 1 d . .
C2 C 0.1901(3) 0.4764(3) 0.38492(11) 0.0366(6) Uani 1 d . .
C3 C 0.1837(4) 0.3562(3) 0.36160(13) 0.0512(8) Uani 1 d . .
H3 H 0.2416(4) 0.2901(3) 0.38005(13) 0.061 Uiso 1 calc R .
C4 C 0.0931(5) 0.3328(4) 0.31149(14) 0.0617(10) Uani 1 d . .
H4 H 0.0910(5) 0.2517(4) 0.29618(14) 0.074 Uiso 1 calc R .
C5 C 0.0069(4) 0.4288(4) 0.28461(12) 0.0553(9) Uani 1 d . .
C6 C 0.0095(4) 0.5478(4) 0.30674(13) 0.0575(9) Uani 1 d . .
H6 H -0.0499(4) 0.6130(4) 0.28818(13) 0.069 Uiso 1 calc R .
C7 C 0.1001(4) 0.5710(3) 0.35657(13) 0.0489(8) Uani 1 d . .
H7 H 0.1008(4) 0.6524(3) 0.37153(13) 0.059 Uiso 1 calc R .
Cl1 Cl -0.11079(14) 0.40026(13) 0.22161(4) 0.0903(4) Uani 1 d . .
N3 N 0.3012(3) 0.8265(2) 0.45229(10) 0.0390(6) Uani 1 d . .
C8 C 0.3706(4) 0.8210(3) 0.40838(14) 0.0504(8) Uani 1 d . .
H8 H 0.3827(4) 0.7416(3) 0.39297(14) 0.060 Uiso 1 calc R .
C9 C 0.4255(4) 0.9265(4) 0.3845(2) 0.0587(9) Uani 1 d . .
H9 H 0.4715(4) 0.9193(4) 0.3533(2) 0.070 Uiso 1 calc R .
C10 C 0.4101(4) 1.0432(3) 0.4084(2) 0.0609(10) Uani 1 d . .
H10 H 0.4467(4) 1.1166(3) 0.3936(2) 0.073 Uiso 1 calc R .
C11 C 0.3410(4) 1.0511(3) 0.4538(2) 0.0531(9) Uani 1 d . .
H11 H 0.3302(4) 1.1297(3) 0.4701(2) 0.064 Uiso 1 calc R .
C12 C 0.2869(3) 0.9408(3) 0.47539(12) 0.0403(7) Uani 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'
Cl Cl 0.1484 0.1585 '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
N1 Mn1 N1 178.48(12) 5_666 6_565 yes
N1 Mn1 N2 90.80(9) 5_666 2_556 yes
N1 Mn1 N2 88.17(9) 6_565 2_556 yes
N1 Mn1 N2 88.17(9) 5_666 . yes
N1 Mn1 N2 90.80(9) 6_565 . yes
N2 Mn1 N2 94.93(12) 2_556 . yes
N1 Mn1 N3 97.22(9) 5_666 2_556 yes
N1 Mn1 N3 84.03(9) 6_565 2_556 yes
N2 Mn1 N3 97.23(9) 2_556 2_556 yes
N2 Mn1 N3 166.62(9) . 2_556 yes
N1 Mn1 N3 84.03(9) 5_666 . yes
N1 Mn1 N3 97.22(9) 6_565 . yes
N2 Mn1 N3 166.62(9) 2_556 . yes
N2 Mn1 N3 97.23(9) . . yes
N3 Mn1 N3 71.31(13) 2_556 . yes
C1 N1 Mn1 140.4(2) . 5_666 yes
N1 C1 N2 176.2(3) . . yes
C1 N2 C2 116.6(2) . . yes
C1 N2 Mn1 111.3(2) . . yes
C2 N2 Mn1 131.1(2) . . yes
C7 C2 C3 117.4(3) . . ?
C7 C2 N2 119.8(3) . . ?
C3 C2 N2 122.8(3) . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4(2) . . ?
C2 C3 H3 119.4(2) . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2(2) . . ?
C3 C4 H4 120.2(2) . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 Cl1 120.3(3) . . ?
C6 C5 Cl1 119.2(3) . . ?
C7 C6 C5 119.7(3) . . ?
C7 C6 H6 120.1(2) . . ?
C5 C6 H6 120.1(2) . . ?
C6 C7 C2 121.5(3) . . ?
C6 C7 H7 119.3(2) . . ?
C2 C7 H7 119.3(2) . . ?
C8 N3 C12 118.4(3) . . ?
C8 N3 Mn1 122.9(2) . . ?
C12 N3 Mn1 117.6(2) . . ?
N3 C8 C9 123.6(3) . . ?
N3 C8 H8 118.2(2) . . ?
C9 C8 H8 118.2(2) . . ?
C8 C9 C10 117.6(3) . . ?
C8 C9 H9 121.2(2) . . ?
C10 C9 H9 121.2(2) . . ?
C11 C10 C9 119.9(3) . . ?
C11 C10 H10 120.1(2) . . ?
C9 C10 H10 120.1(2) . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 H11 120.3(2) . . ?
C12 C11 H11 120.3(2) . . ?
N3 C12 C11 121.1(3) . . ?
N3 C12 C12 116.0(2) . 2_556 ?
C11 C12 C12 122.8(2) . 2_556 ?
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
Mn1 Mn1 5.328(2) 5_666 yes
Mn1 N1 2.222(3) 5_666 yes
Mn1 N1 2.222(3) 6_565 yes
Mn1 N2 2.253(2) 2_556 yes
Mn1 N2 2.253(2) . yes
Mn1 N3 2.284(2) 2_556 yes
Mn1 N3 2.284(2) . yes
N1 C1 1.169(4) . yes
N1 Mn1 2.222(3) 5_666 yes
C1 N2 1.292(4) . yes
N2 C2 1.412(3) . yes
C2 C7 1.379(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.379(5) . ?
C3 H3 0.93 . ?
C4 C5 1.359(5) . ?
C4 H4 0.93 . ?
C5 C6 1.362(5) . ?
C5 Cl1 1.746(3) . ?
C6 C7 1.374(5) . ?
C6 H6 0.93 . ?
C7 H7 0.93 . ?
N3 C8 1.330(4) . ?
N3 C12 1.343(4) . ?
C8 C9 1.375(5) . ?
C8 H8 0.93 . ?
C9 C10 1.376(5) . ?
C9 H9 0.93 . ?
C10 C11 1.361(5) . ?
C10 H10 0.93 . ?
C11 C12 1.388(4) . ?
C11 H11 0.93 . ?
C12 C12 1.469(6) 2_556 ?
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
Mn1 N1 C1 N2 -59.2(49) 5_666 . . . ?
N1 C1 N2 C2 178.1(1000) . . . . ?
N1 C1 N2 Mn1 -11.7(48) . . . . ?
N1 Mn1 N2 C1 37.8(2) 5_666 . . . ?
N1 Mn1 N2 C1 -141.1(2) 6_565 . . . ?
N2 Mn1 N2 C1 -52.8(2) 2_556 . . . ?
N3 Mn1 N2 C1 152.0(3) 2_556 . . . ?
N3 Mn1 N2 C1 121.6(2) . . . . ?
N1 Mn1 N2 C2 -153.8(2) 5_666 . . . ?
N1 Mn1 N2 C2 27.3(2) 6_565 . . . ?
N2 Mn1 N2 C2 115.5(3) 2_556 . . . ?
N3 Mn1 N2 C2 -39.7(5) 2_556 . . . ?
N3 Mn1 N2 C2 -70.1(2) . . . . ?
C1 N2 C2 C7 -164.0(3) . . . . ?
Mn1 N2 C2 C7 28.1(4) . . . . ?
C1 N2 C2 C3 16.8(4) . . . . ?
Mn1 N2 C2 C3 -151.1(2) . . . . ?
C7 C2 C3 C4 1.2(5) . . . . ?
N2 C2 C3 C4 -179.6(3) . . . . ?
C2 C3 C4 C5 -0.7(6) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C3 C4 C5 Cl1 -179.0(3) . . . . ?
C4 C5 C6 C7 0.1(6) . . . . ?
Cl1 C5 C6 C7 179.2(3) . . . . ?
C5 C6 C7 C2 0.4(5) . . . . ?
C3 C2 C7 C6 -1.0(5) . . . . ?
N2 C2 C7 C6 179.8(3) . . . . ?
N1 Mn1 N3 C8 71.6(2) 5_666 . . . ?
N1 Mn1 N3 C8 -107.6(2) 6_565 . . . ?
N2 Mn1 N3 C8 139.3(4) 2_556 . . . ?
N2 Mn1 N3 C8 -15.8(2) . . . . ?
N3 Mn1 N3 C8 171.3(3) 2_556 . . . ?
N1 Mn1 N3 C12 -95.9(2) 5_666 . . . ?
N1 Mn1 N3 C12 85.0(2) 6_565 . . . ?
N2 Mn1 N3 C12 -28.2(5) 2_556 . . . ?
N2 Mn1 N3 C12 176.7(2) . . . . ?
N3 Mn1 N3 C12 3.83(14) 2_556 . . . ?
C12 N3 C8 C9 -1.6(5) . . . . ?
Mn1 N3 C8 C9 -168.9(3) . . . . ?
N3 C8 C9 C10 1.4(5) . . . . ?
C8 C9 C10 C11 -0.6(5) . . . . ?
C9 C10 C11 C12 0.0(5) . . . . ?
C8 N3 C12 C11 0.9(4) . . . . ?
Mn1 N3 C12 C11 168.9(2) . . . . ?
C8 N3 C12 C12 -178.4(3) . . . 2_556 ?
Mn1 N3 C12 C12 -10.4(4) . . . 2_556 ?
C10 C11 C12 N3 -0.1(5) . . . . ?
C10 C11 C12 C12 179.1(3) . . . 2_556 ?
