#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312966.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_4312966
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            'C38 H30 Cl2 Mn N6 O4'
_chemical_formula_weight         760.52
_chemical_name_common            '[Mn(4-Bzpy)2(3-Cl-C6H4-NCN)2(H2O)2]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.630(3)
_cell_length_b                   12.559(5)
_cell_length_c                   18.886(7)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      9.4
_cell_volume                     1807.3(12)
_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      300(2)
_diffrn_measurement_device       'mod. STOE 4-circle diffractometer'
_diffrn_measurement_method       'Omega_scan; delta Omega: 1.20 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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3831
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        6
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       prism
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.144
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_obs          0.0473
_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)+(0.0371P)²+0.7068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1196
_refine_ls_wR_factor_obs         0.1001
_reflns_number_observed          2411
_reflns_number_total             3207
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic025931l_s1_1.cif
_cod_data_source_block           aens2b
_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^)+(0.0371P)^2^+0.7068P] 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^)+(0.0371P)^2^+0.7068P] 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               4312966
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn 0.0000 0.0000 0.0000 0.0356(2) Uani 1 d S .
Cl1 Cl 0.1384(2) 0.21885(9) 0.32562(5) 0.0949(4) Uani 1 d . .
O1 O 0.2791(3) 0.0069(2) -0.00815(13) 0.0535(6) Uani 1 d D .
N3 N 0.0044(3) 0.3507(2) 0.07027(12) 0.0435(6) Uani 1 d . .
N1 N 0.0463(3) -0.0662(2) 0.11807(12) 0.0446(6) Uani 1 d . .
C3 C 0.1040(5) -0.1479(3) 0.2550(2) 0.0532(8) Uani 1 d . .
C14 C 0.0281(4) 0.3720(2) 0.14346(15) 0.0397(7) Uani 1 d . .
C7 C 0.1630(5) -0.1326(3) 0.3917(2) 0.0574(9) Uani 1 d . .
C15 C 0.0720(4) 0.2924(2) 0.1932(2) 0.0485(8) Uani 1 d . .
H15 H 0.0869(4) 0.2222(2) 0.1790(2) 0.058 Uiso 1 calc R .
C16 C 0.0928(5) 0.3202(3) 0.2640(2) 0.0567(9) Uani 1 d . .
C13 C 0.0037(4) 0.2516(2) 0.05223(14) 0.0389(7) Uani 1 d . .
C17 C 0.0770(5) 0.4223(3) 0.2870(2) 0.0654(10) Uani 1 d . .
H17 H 0.0939(5) 0.4392(3) 0.3348(2) 0.079 Uiso 1 calc R .
C8 C 0.1257(6) -0.1752(3) 0.4578(2) 0.0812(12) Uani 1 d . .
H8 H 0.0754(6) -0.2424(3) 0.4606(2) 0.097 Uiso 1 calc R .
N2 N 0.0007(4) 0.1637(2) 0.03418(13) 0.0526(7) Uani 1 d . .
C9 C 0.1638(7) -0.1171(4) 0.5187(2) 0.0918(15) Uani 1 d . .
H9 H 0.1385(7) -0.1452(4) 0.5626(2) 0.110 Uiso 1 calc R .
C2 C 0.1694(5) -0.1983(3) 0.1968(2) 0.0565(9) Uani 1 d . .
H2 H 0.2329(5) -0.2612(3) 0.2025(2) 0.068 Uiso 1 calc R .
C19 C 0.0109(4) 0.4756(2) 0.1668(2) 0.0526(8) Uani 1 d . .
H19 H -0.0174(4) 0.5292(2) 0.1342(2) 0.063 Uiso 1 calc R .
C12 C 0.2369(5) -0.0324(3) 0.3892(2) 0.0603(9) Uani 1 d . .
H12 H 0.2609(5) -0.0026(3) 0.3457(2) 0.072 Uiso 1 calc R .
C1 C 0.1396(4) -0.1547(2) 0.1302(2) 0.0517(8) Uani 1 d . .
H1 H 0.1870(4) -0.1887(2) 0.0919(2) 0.062 Uiso 1 calc R .
C5 C -0.0182(4) -0.0188(2) 0.1742(2) 0.0477(7) Uani 1 d . .
H5 H -0.0845(4) 0.0428(2) 0.1670(2) 0.057 Uiso 1 calc R .
C10 C 0.2384(7) -0.0186(4) 0.5148(2) 0.0906(14) Uani 1 d . .
H10 H 0.2642(7) 0.0198(4) 0.5562(2) 0.109 Uiso 1 calc R .
C18 C 0.0351(5) 0.5003(3) 0.2374(2) 0.0650(10) Uani 1 d . .
H18 H 0.0230(5) 0.5705(3) 0.2520(2) 0.078 Uiso 1 calc R .
C4 C 0.0086(4) -0.0566(3) 0.2427(2) 0.0529(8) Uani 1 d . .
H4 H -0.0378(4) -0.0202(3) 0.2803(2) 0.063 Uiso 1 calc R .
O2 O 0.1283(6) -0.2942(2) 0.3314(2) 0.139(2) Uani 1 d . .
C11 C 0.2755(6) 0.0241(3) 0.4508(2) 0.0788(12) Uani 1 d . .
H11 H 0.3268(6) 0.0912(3) 0.4487(2) 0.095 Uiso 1 calc R .
C6 C 0.1319(6) -0.1993(3) 0.3277(2) 0.0720(11) Uani 1 d . .
H6 H 0.3421(41) -0.0417(23) -0.0199(18) 0.064(8) Uiso 1 d D .
H7 H 0.3362(41) 0.0550(23) 0.0119(16) 0.064(8) Uiso 1 d 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'
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'
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
O1 Mn1 O1 180.0 3 . ?
O1 Mn1 N2 90.22(10) 3 . yes
O1 Mn1 N2 89.78(10) . . ?
O1 Mn1 N2 89.78(10) 3 3 ?
O1 Mn1 N2 90.22(10) . 3 ?
N2 Mn1 N2 180.0 . 3 ?
O1 Mn1 N1 91.02(9) 3 . yes
O1 Mn1 N1 88.98(9) . . ?
N2 Mn1 N1 93.13(9) . . yes
N2 Mn1 N1 86.87(9) 3 . ?
O1 Mn1 N1 88.98(9) 3 3 ?
O1 Mn1 N1 91.02(9) . 3 ?
N2 Mn1 N1 86.87(9) . 3 ?
N2 Mn1 N1 93.13(9) 3 3 ?
N1 Mn1 N1 180.0 . 3 ?
Mn1 O1 H6 126.3(25) . . ?
Mn1 O1 H7 119.9(24) . . ?
H6 O1 H7 111.6(33) . . ?
C13 N3 C14 116.1(2) . . yes
C5 N1 C1 116.9(3) . . ?
C5 N1 Mn1 123.0(2) . . ?
C1 N1 Mn1 120.2(2) . . ?
C4 C3 C2 117.3(3) . . ?
C4 C3 C6 123.6(3) . . ?
C2 C3 C6 118.9(3) . . ?
C19 C14 C15 118.8(3) . . ?
C19 C14 N3 118.8(3) . . ?
C15 C14 N3 122.5(3) . . ?
C12 C7 C8 118.7(3) . . ?
C12 C7 C6 122.5(3) . . ?
C8 C7 C6 118.7(3) . . ?
C16 C15 C14 118.7(3) . . ?
C16 C15 H15 120.7(2) . . ?
C14 C15 H15 120.7(2) . . ?
C17 C16 C15 122.6(3) . . ?
C17 C16 Cl1 119.5(3) . . ?
C15 C16 Cl1 117.9(3) . . ?
N2 C13 N3 178.0(3) . . yes
C16 C17 C18 118.2(3) . . ?
C16 C17 H17 120.9(2) . . ?
C18 C17 H17 120.9(2) . . ?
C9 C8 C7 119.8(4) . . ?
C9 C8 H8 120.1(3) . . ?
C7 C8 H8 120.1(2) . . ?
C13 N2 Mn1 178.9(3) . . yes
C10 C9 C8 120.3(4) . . ?
C10 C9 H9 119.9(3) . . ?
C8 C9 H9 119.9(3) . . ?
C1 C2 C3 119.5(3) . . ?
C1 C2 H2 120.2(2) . . ?
C3 C2 H2 120.2(2) . . ?
C18 C19 C14 120.9(3) . . ?
C18 C19 H19 119.6(2) . . ?
C14 C19 H19 119.6(2) . . ?
C11 C12 C7 120.6(4) . . ?
C11 C12 H12 119.7(2) . . ?
C7 C12 H12 119.7(2) . . ?
N1 C1 C2 123.3(3) . . ?
N1 C1 H1 118.3(2) . . ?
C2 C1 H1 118.3(2) . . ?
N1 C5 C4 123.2(3) . . ?
N1 C5 H5 118.4(2) . . ?
C4 C5 H5 118.4(2) . . ?
C9 C10 C11 120.6(4) . . ?
C9 C10 H10 119.7(3) . . ?
C11 C10 H10 119.7(3) . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.6(2) . . ?
C17 C18 H18 119.6(2) . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.2(2) . . ?
C5 C4 H4 120.2(2) . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.0(3) . . ?
C12 C11 H11 120.0(2) . . ?
O2 C6 C7 121.4(3) . . ?
O2 C6 C3 118.2(3) . . ?
C7 C6 C3 120.4(3) . . ?
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 O1 2.145(2) 3 yes
Mn1 O1 2.145(2) . yes
Mn1 N2 2.154(3) . yes
Mn1 N2 2.154(3) 3 yes
Mn1 N1 2.389(2) . yes
Mn1 N1 2.389(2) 3 yes
Cl1 C16 1.747(3) . ?
O1 H6 0.81(2) . yes
O1 H7 0.83(2) . yes
N3 C13 1.290(4) . yes
N3 C14 1.410(4) . yes
N1 C5 1.333(4) . ?
N1 C1 1.333(4) . ?
C3 C4 1.371(4) . ?
C3 C2 1.384(4) . ?
C3 C6 1.523(4) . ?
C14 C19 1.382(4) . ?
C14 C15 1.401(4) . ?
C7 C12 1.382(5) . ?
C7 C8 1.401(5) . ?
C7 C6 1.478(5) . ?
C15 C16 1.383(4) . ?
C15 H15 0.93 . ?
C16 C17 1.361(5) . ?
C13 N2 1.156(3) . yes
C17 C18 1.381(5) . ?
C17 H17 0.93 . ?
C8 C9 1.380(6) . ?
C8 H8 0.93 . ?
C9 C10 1.365(6) . ?
C9 H9 0.93 . ?
C2 C1 1.379(4) . ?
C2 H2 0.93 . ?
C19 C18 1.372(4) . ?
C19 H19 0.93 . ?
C12 C11 1.381(5) . ?
C12 H12 0.93 . ?
C1 H1 0.93 . ?
C5 C4 1.384(4) . ?
C5 H5 0.93 . ?
C10 C11 1.366(6) . ?
C10 H10 0.93 . ?
C18 H18 0.93 . ?
C4 H4 0.93 . ?
O2 C6 1.194(4) . ?
C11 H11 0.93 . ?
N3 O1 2.856(5) 2_555 yes
N3 O1 2.843(5) 4_565 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Mn1 N1 C5 -56.9(2) 3 . . . ?
O1 Mn1 N1 C5 123.1(2) . . . . ?
N2 Mn1 N1 C5 33.4(2) . . . . ?
N2 Mn1 N1 C5 -146.6(2) 3 . . . ?
N1 Mn1 N1 C5 -175.2(261) 3 . . . ?
O1 Mn1 N1 C1 122.8(2) 3 . . . ?
O1 Mn1 N1 C1 -57.2(2) . . . . ?
N2 Mn1 N1 C1 -146.9(2) . . . . ?
N2 Mn1 N1 C1 33.1(2) 3 . . . ?
N1 Mn1 N1 C1 4.5(261) 3 . . . ?
C13 N3 C14 C19 -173.0(3) . . . . ?
C13 N3 C14 C15 8.3(4) . . . . ?
C19 C14 C15 C16 1.4(5) . . . . ?
N3 C14 C15 C16 -180.0(3) . . . . ?
C14 C15 C16 C17 -1.9(5) . . . . ?
C14 C15 C16 Cl1 177.4(2) . . . . ?
C14 N3 C13 N2 160.4(94) . . . . ?
C15 C16 C17 C18 1.3(6) . . . . ?
Cl1 C16 C17 C18 -177.9(3) . . . . ?
C12 C7 C8 C9 -0.3(6) . . . . ?
C6 C7 C8 C9 176.0(4) . . . . ?
N3 C13 N2 Mn1 99.5(145) . . . . ?
O1 Mn1 N2 C13 -169.3(1000) 3 . . . ?
O1 Mn1 N2 C13 10.7(123) . . . . ?
N2 Mn1 N2 C13 -64.3(143) 3 . . . ?
N1 Mn1 N2 C13 99.6(123) . . . . ?
N1 Mn1 N2 C13 -80.4(123) 3 . . . ?
C7 C8 C9 C10 -0.3(7) . . . . ?
C4 C3 C2 C1 1.2(5) . . . . ?
C6 C3 C2 C1 177.7(3) . . . . ?
C15 C14 C19 C18 -0.4(5) . . . . ?
N3 C14 C19 C18 -179.1(3) . . . . ?
C8 C7 C12 C11 0.9(6) . . . . ?
C6 C7 C12 C11 -175.3(4) . . . . ?
C5 N1 C1 C2 0.7(5) . . . . ?
Mn1 N1 C1 C2 -179.0(2) . . . . ?
C3 C2 C1 N1 -1.6(5) . . . . ?
C1 N1 C5 C4 0.5(4) . . . . ?
Mn1 N1 C5 C4 -179.8(2) . . . . ?
C8 C9 C10 C11 0.3(7) . . . . ?
C14 C19 C18 C17 -0.1(5) . . . . ?
C16 C17 C18 C19 -0.3(6) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C6 C3 C4 C5 -176.3(3) . . . . ?
N1 C5 C4 C3 -0.8(5) . . . . ?
C9 C10 C11 C12 0.2(7) . . . . ?
C7 C12 C11 C10 -0.9(6) . . . . ?
C12 C7 C6 O2 153.2(5) . . . . ?
C8 C7 C6 O2 -23.0(7) . . . . ?
C12 C7 C6 C3 -26.6(6) . . . . ?
C8 C7 C6 C3 157.2(4) . . . . ?
C4 C3 C6 O2 140.8(5) . . . . ?
C2 C3 C6 O2 -35.4(6) . . . . ?
C4 C3 C6 C7 -39.4(5) . . . . ?
C2 C3 C6 C7 144.5(4) . . . . ?
