#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/83/2218345.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_2218345
loop_
_publ_author_name
'Sun, Zhen-Hai'
'Yang, Gui-Bin'
'Meng, Ling-Bo'
'Chen, Shen'
_publ_section_title
Diaqua-1κO,3κO-di-μ-cyanido-1:2κ²N:C;2:3κ²C:N-dicyanido-2κ²N-bis{4,4'-dibromo-2,2'-[propane-1,2-diylbis(nitrilomethylidyne)]diphenolato}-1κ⁴O,N,N',O';3κ⁴O,N,N',O'-1,3-dimanganese(III)-2-nickel(II)
_journal_coeditor_code           CF2192
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m783
_journal_paper_doi               10.1107/S1600536808012749
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Mn2 Ni (C17 H14 Br2 N2 O2)2 (C N)4 (H2 O)2]'
_chemical_formula_moiety         'C38 H32 Br4 Mn2 N8 Ni O6'
_chemical_formula_sum            'C38 H32 Br4 Mn2 N8 Ni O6'
_chemical_formula_weight         1184.95
_chemical_name_systematic
;
Diaqua-1\kO,3\kO-di-μ-cyanido-1:2κ²N:C;2:3κ²C:N-dicyanido-2κ²N-
bis{4,4'-dibromo-2,2'-[propane-1,2-diylbis(nitrilomethylidyne)]diphenolato}-
1κ⁴O,N,N',O';3κ⁴O,N,N',O'-1,3-dimanganese(III)-2-nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 112.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.619(2)
_cell_length_b                   13.514(3)
_cell_length_c                   14.741(3)
_cell_measurement_reflns_used    3712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      3.01
_cell_volume                     2145.5(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0849
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13467
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.793
_exptl_absorpt_correction_T_max  0.7004
_exptl_absorpt_correction_T_min  0.5970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.686
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0645
_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)+(0.085P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1749
_reflns_number_gt                2268
_reflns_number_total             3712
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf2192.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2145.5(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218345
_cod_database_fobs_code          2218345
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
Ni Ni1 0.0000 1.0000 0.0000 0.0349(4) Uani d S 1
Mn Mn1 0.29546(11) 0.95323(8) 0.36729(8) 0.0306(4) Uani d . 1
Br Br2 -0.07326(10) 1.37224(7) 0.43825(7) 0.0583(4) Uani d . 1
Br Br4 0.75942(10) 0.61247(7) 0.30713(8) 0.0636(4) Uani d . 1
C C1 0.1213(8) 0.9936(5) 0.1259(5) 0.036(2) Uani d . 1
C C2 -0.0637(8) 0.8806(6) 0.0275(6) 0.039(2) Uani d . 1
C C3 0.2230(8) 1.1458(5) 0.4133(5) 0.035(2) Uani d . 1
C C4 0.2475(8) 1.2492(5) 0.4247(5) 0.0338(19) Uani d . 1
H H4 0.3241 1.2728 0.4279 0.041 Uiso calc R 1
C C5 0.1609(9) 1.3147(6) 0.4311(6) 0.043(2) Uani d . 1
H H5 0.1781 1.3821 0.4359 0.052 Uiso calc R 1
C C6 0.0470(9) 1.2810(6) 0.4305(6) 0.043(2) Uani d . 1
C C7 0.0187(9) 1.1818(6) 0.4197(6) 0.046(2) Uani d . 1
H H7 -0.0578 1.1601 0.4184 0.056 Uiso calc R 1
C C8 0.1033(8) 1.1135(5) 0.4107(6) 0.038(2) Uani d . 1
C C9 0.0682(8) 1.0107(6) 0.3967(6) 0.037(2) Uani d . 1
H H9 -0.0076 0.9939 0.4003 0.045 Uiso calc R 1
C C10 0.0874(10) 0.8352(6) 0.3699(9) 0.070(3) Uani d . 1
H H10A 0.1148 0.8044 0.4340 0.084 Uiso calc R 1
H H10B -0.0026 0.8335 0.3419 0.084 Uiso calc R 1
C C11 0.1358(9) 0.7815(6) 0.3084(9) 0.069(3) Uani d . 1
H H11 0.0896 0.8087 0.2432 0.082 Uiso calc R 1
C C12 0.1046(9) 0.6736(6) 0.2966(8) 0.063(3) Uani d . 1
H H12A 0.1564 0.6386 0.3541 0.094 Uiso calc R 1
H H12B 0.1185 0.6485 0.2406 0.094 Uiso calc R 1
H H12C 0.0190 0.6645 0.2874 0.094 Uiso calc R 1
C C13 0.3444(7) 0.7543(5) 0.3197(5) 0.034(2) Uani d . 1
H H13 0.3200 0.6888 0.3050 0.041 Uiso calc R 1
C C14 0.4691(7) 0.7788(5) 0.3300(5) 0.035(2) Uani d . 1
C C15 0.5439(8) 0.7030(6) 0.3193(5) 0.039(2) Uani d . 1
H H15 0.5142 0.6384 0.3117 0.047 Uiso calc R 1
C C16 0.6589(9) 0.7208(7) 0.3196(6) 0.050(3) Uani d . 1
C C17 0.7050(9) 0.8158(7) 0.3290(6) 0.050(2) Uani d . 1
H H17 0.7826 0.8279 0.3265 0.060 Uiso calc R 1
C C18 0.6340(8) 0.8932(6) 0.3422(6) 0.041(2) Uani d . 1
H H18 0.6660 0.9571 0.3508 0.049 Uiso calc R 1
C C19 0.5152(8) 0.8769(6) 0.3428(5) 0.034(2) Uani d . 1
N N1 0.1906(6) 0.9902(4) 0.2061(4) 0.0384(18) Uani d . 1
N N2 -0.0940(7) 0.8037(5) 0.0442(5) 0.048(2) Uani d . 1
N N3 0.1310(6) 0.9397(5) 0.3797(5) 0.0411(18) Uani d . 1
N N4 0.2646(6) 0.8130(4) 0.3287(4) 0.0316(16) Uani d . 1
O O1 0.4523(5) 0.9530(3) 0.3561(3) 0.0328(13) Uani d . 1
O O2 0.3094(5) 1.0873(3) 0.4049(4) 0.0327(13) Uani d . 1
O O3 0.3787(5) 0.9022(4) 0.5249(4) 0.0368(14) Uani d D 1
H H1W 0.434(5) 0.942(4) 0.552(7) 0.080 Uiso d D 1
H H2W 0.398(7) 0.8437(15) 0.533(7) 0.080 Uiso d 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'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 '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
C1 Ni1 C1 . 3_575 180
C1 Ni1 C2 . 3_575 92.5(3)
C1 Ni1 C2 3_575 3_575 87.5(3)
C1 Ni1 C2 . . 87.5(3)
C1 Ni1 C2 3_575 . 92.5(3)
C2 Ni1 C2 3_575 . 180
O2 Mn1 O1 . . 92.8(2)
O2 Mn1 N4 . . 174.4(3)
O1 Mn1 N4 . . 92.9(2)
O2 Mn1 N3 . . 92.3(2)
O1 Mn1 N3 . . 174.6(2)
N4 Mn1 N3 . . 82.0(3)
O2 Mn1 O3 . . 92.0(2)
O1 Mn1 O3 . . 92.0(2)
N4 Mn1 O3 . . 88.0(2)
N3 Mn1 O3 . . 86.2(3)
O2 Mn1 N1 . . 92.8(2)
O1 Mn1 N1 . . 93.7(2)
N4 Mn1 N1 . . 86.7(2)
N3 Mn1 N1 . . 87.7(3)
O3 Mn1 N1 . . 172.4(2)
N1 C1 Ni1 . . 175.8(8)
N2 C2 Ni1 . . 174.3(8)
O2 C3 C4 . . 118.2(7)
O2 C3 C8 . . 125.2(7)
C4 C3 C8 . . 116.6(7)
C5 C4 C3 . . 121.5(8)
C5 C4 H4 . . 119.2
C3 C4 H4 . . 119.2
C4 C5 C6 . . 120.5(7)
C4 C5 H5 . . 119.8
C6 C5 H5 . . 119.8
C7 C6 C5 . . 120.2(8)
C7 C6 Br2 . . 119.4(7)
C5 C6 Br2 . . 120.3(6)
C6 C7 C8 . . 120.8(9)
C6 C7 H7 . . 119.6
C8 C7 H7 . . 119.6
C7 C8 C9 . . 118.8(8)
C7 C8 C3 . . 120.4(7)
C9 C8 C3 . . 120.8(7)
N3 C9 C8 . . 126.6(8)
N3 C9 H9 . . 116.7
C8 C9 H9 . . 116.7
C11 C10 N3 . . 109.9(8)
C11 C10 H10A . . 109.7
N3 C10 H10A . . 109.7
C11 C10 H10B . . 109.7
N3 C10 H10B . . 109.7
H10A C10 H10B . . 108.2
C10 C11 N4 . . 109.6(8)
C10 C11 C12 . . 115.6(9)
N4 C11 C12 . . 119.2(8)
C10 C11 H11 . . 103.4
N4 C11 H11 . . 103.4
C12 C11 H11 . . 103.4
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
N4 C13 C14 . . 126.4(7)
N4 C13 H13 . . 116.8
C14 C13 H13 . . 116.8
C15 C14 C19 . . 119.0(8)
C15 C14 C13 . . 117.8(7)
C19 C14 C13 . . 123.1(7)
C16 C15 C14 . . 121.7(8)
C16 C15 H15 . . 119.1
C14 C15 H15 . . 119.1
C15 C16 C17 . . 120.8(9)
C15 C16 Br4 . . 119.8(7)
C17 C16 Br4 . . 119.4(8)
C16 C17 C18 . . 119.0(9)
C16 C17 H17 . . 120.5
C18 C17 H17 . . 120.5
C17 C18 C19 . . 121.4(8)
C17 C18 H18 . . 119.3
C19 C18 H18 . . 119.3
O1 C19 C18 . . 118.7(7)
O1 C19 C14 . . 123.2(8)
C18 C19 C14 . . 118.1(7)
C1 N1 Mn1 . . 165.7(7)
C9 N3 C10 . . 121.9(8)
C9 N3 Mn1 . . 125.6(6)
C10 N3 Mn1 . . 112.4(5)
C13 N4 C11 . . 121.7(6)
C13 N4 Mn1 . . 124.9(6)
C11 N4 Mn1 . . 113.3(5)
C19 O1 Mn1 . . 128.4(5)
C3 O2 Mn1 . . 128.3(5)
Mn1 O3 H1W . . 105(7)
Mn1 O3 H2W . . 116(7)
H1W O3 H2W . . 116(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 C1 . 1.865(8)
Ni1 C1 3_575 1.865(8)
Ni1 C2 3_575 1.882(9)
Ni1 C2 . 1.882(9)
Mn1 O2 . 1.884(5)
Mn1 O1 . 1.890(6)
Mn1 N4 . 1.973(6)
Mn1 N3 . 1.995(7)
Mn1 O3 . 2.264(5)
Mn1 N1 . 2.282(6)
Br2 C6 . 1.899(9)
Br4 C16 . 1.925(9)
C1 N1 . 1.154(9)
C2 N2 . 1.153(9)
C3 O2 . 1.319(9)
C3 C4 . 1.423(10)
C3 C8 . 1.443(12)
C4 C5 . 1.370(11)
C4 H4 . 0.930
C5 C6 . 1.397(12)
C5 H5 . 0.930
C6 C7 . 1.375(11)
C7 C8 . 1.390(11)
C7 H7 . 0.930
C8 C9 . 1.442(10)
C9 N3 . 1.286(10)
C9 H9 . 0.930
C10 C11 . 1.431(13)
C10 N3 . 1.489(10)
C10 H10A . 0.970
C10 H10B . 0.970
C11 N4 . 1.475(11)
C11 C12 . 1.497(11)
C11 H11 . 0.980
C12 H12A . 0.960
C12 H12B . 0.960
C12 H12C . 0.960
C13 N4 . 1.265(9)
C13 C14 . 1.438(11)
C13 H13 . 0.930
C14 C15 . 1.389(11)
C14 C19 . 1.415(10)
C15 C16 . 1.356(12)
C15 H15 . 0.930
C16 C17 . 1.378(12)
C17 C18 . 1.391(12)
C17 H17 . 0.930
C18 C19 . 1.401(12)
C18 H18 . 0.930
C19 O1 . 1.319(9)
O3 H1W . 0.82(7)
O3 H2W . 0.82(4)
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
O3 H1W O1 3_676 0.82(7) 2.06(7) 2.860(7) 165(10)
O3 H2W N2 4_676 0.82(4) 2.00(2) 2.803(8) 167(8)
