#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/57/1505722.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_1505722
loop_
_publ_author_name
'Sarkar, Sumana'
'Datta, Ayan'
'Mondal, Amrita'
'Chopra, Deepak'
'Ribas, Joan'
'Rajak, Kajal Krishna'
'Sairam S M, Sairam'
'Pati, Swapan K.'
_publ_section_title
;
 Competing magnetic interactions in a dinuclear Ni(II) complex:
 antiferromagnetic O-H...O moiety and ferromagnetic N3- ligand.
;
_journal_issue                   1
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              12
_journal_page_last               15
_journal_paper_doi               10.1021/jp0556963
_journal_volume                  110
_journal_year                    2006
_chemical_formula_sum            'C36 H49 Cl N12 Ni2 O6'
_chemical_formula_weight         898.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_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            8
_cell_length_a                   16.345(4)
_cell_length_b                   17.334(4)
_cell_length_c                   14.973(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.7
_cell_volume                     4242.2(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.740
_diffrn_measured_fraction_theta_max 0.740
_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  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31629
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.8233
_exptl_absorpt_correction_T_min  0.7512
_exptl_absorpt_process_details   '(SADABS; Sheldrik, 1997)'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.1057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0724P)²+7.7341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2139
_reflns_number_gt                3468
_reflns_number_total             4604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp0556963si20051006_102239.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_sg_symbol_H-M      Pbcn
_cod_database_code               1505722
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x, y-1/2, z'
'x-1/2, -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
C1 C 0.9029(4) 0.6374(4) 0.4268(3) 0.0482(15) Uani 1 1 d .
C2 C 0.9787(4) 0.6658(5) 0.4164(4) 0.066(2) Uani 1 1 d .
H2 H 0.9923 0.7176 0.4227 0.079 Uiso 1 1 calc R
C3 C 1.0368(4) 0.6050(6) 0.3942(5) 0.084(3) Uani 1 1 d .
H3 H 1.0909 0.6204 0.3867 0.100 Uiso 1 1 calc R
C4 C 1.0194(5) 0.5174(6) 0.3814(5) 0.082(3) Uani 1 1 d .
C5 C 0.9452(5) 0.4893(5) 0.3922(5) 0.074(2) Uani 1 1 d .
H5 H 0.9324 0.4374 0.3852 0.089 Uiso 1 1 calc R
C6 C 0.8861(4) 0.5474(4) 0.4160(4) 0.0571(17) Uani 1 1 d .
C7 C 0.8075(4) 0.5097(4) 0.4351(4) 0.0617(18) Uani 1 1 d .
H7A H 0.8085 0.4569 0.4139 0.074 Uiso 1 1 calc R
H7B H 0.7978 0.5090 0.4991 0.074 Uiso 1 1 calc R
C8 C 0.6683(5) 0.5099(4) 0.4175(4) 0.0651(19) Uani 1 1 d .
H8A H 0.6715 0.4940 0.4795 0.078 Uiso 1 1 calc R
H8B H 0.6597 0.4649 0.3802 0.078 Uiso 1 1 calc R
C9 C 0.6007(4) 0.5700(5) 0.4034(4) 0.063(2) Uani 1 1 d .
C10 C 0.5257(6) 0.5376(7) 0.3948(6) 0.102(3) Uani 1 1 d .
H10 H 0.5149 0.4850 0.3923 0.122 Uiso 1 1 calc R
C11 C 0.4656(6) 0.5976(9) 0.3903(6) 0.118(4) Uani 1 1 d .
H11 H 0.4116 0.5817 0.3843 0.141 Uiso 1 1 calc R
C12 C 0.4801(5) 0.6869(7) 0.3944(6) 0.104(4) Uani 1 1 d .
H12 H 0.4360 0.7207 0.3924 0.125 Uiso 1 1 calc R
C13 C 0.5553(4) 0.7137(5) 0.4007(4) 0.068(2) Uani 1 1 d .
H13 H 0.5675 0.7661 0.4018 0.082 Uiso 1 1 calc R
C14 C 0.7490(5) 0.5450(5) 0.3002(4) 0.073(2) Uani 1 1 d .
H14A H 0.6958 0.5348 0.2739 0.087 Uiso 1 1 calc R
H14B H 0.7851 0.5024 0.2858 0.087 Uiso 1 1 calc R
C15 C 0.7854(6) 0.6238(5) 0.2621(5) 0.091(3) Uani 1 1 d .
H15A H 0.7814 0.6206 0.1975 0.109 Uiso 1 1 calc R
H15B H 0.8433 0.6236 0.2763 0.109 Uiso 1 1 calc R
C16 C 0.8099(5) 0.7785(5) 0.2751(4) 0.084(3) Uani 1 1 d .
H16A H 0.8612 0.7686 0.3043 0.127 Uiso 1 1 calc R
H16B H 0.7856 0.8241 0.2999 0.127 Uiso 1 1 calc R
H16C H 0.8191 0.7858 0.2124 0.127 Uiso 1 1 calc R
C17 C 0.6819(5) 0.7326(6) 0.2434(4) 0.099(3) Uani 1 1 d .
H17A H 0.6404 0.6935 0.2470 0.149 Uiso 1 1 calc R
H17B H 0.6957 0.7415 0.1819 0.149 Uiso 1 1 calc R
H17C H 0.6618 0.7795 0.2694 0.149 Uiso 1 1 calc R
C18 C 1.0829(6) 0.4522(7) 0.3562(6) 0.125(4) Uani 1 1 d .
H18A H 1.1362 0.4747 0.3488 0.187 Uiso 1 1 calc R
H18B H 1.0665 0.4280 0.3014 0.187 Uiso 1 1 calc R
H18C H 1.0847 0.4144 0.4030 0.187 Uiso 1 1 calc R
Cl1 Cl 0.77107(19) 0.7500 0.0000 0.0818(9) Uani 1 2 d S
N1 N 0.7419(3) 0.5524(3) 0.3903(3) 0.0491(13) Uani 1 1 d .
N2 N 0.6144(3) 0.6569(4) 0.4056(3) 0.0531(14) Uani 1 1 d .
N3 N 0.7513(3) 0.7083(3) 0.2896(3) 0.0506(13) Uani 1 1 d .
N4 N 0.7169(3) 0.6782(3) 0.5504(3) 0.0411(11) Uani 1 1 d .
N5 N 0.6932(3) 0.6186(3) 0.5903(3) 0.0538(13) Uani 1 1 d .
N6 N 0.6693(6) 0.5618(5) 0.6291(4) 0.111(3) Uani 1 1 d .
Ni1 Ni 0.73153(4) 0.68747(4) 0.41820(4) 0.0370(3) Uani 1 1 d .
O1 O 0.8463(2) 0.6964(2) 0.4453(2) 0.0452(10) Uani 1 1 d .
O2 O 0.8091(6) 0.7079(6) -0.0605(5) 0.159(4) Uani 1 1 d .
O3 O 0.7681(9) 0.6672(10) 0.0501(8) 0.252(7) Uani 1 1 d .
O4 O 0.6931(8) 0.7500 0.0000 0.221(8) Uani 1 2 d S
H1A H 0.856(7) 0.7500 0.5000 0.12(4) Uiso 1 2 d S
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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 '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'
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
C2 C1 O1 111.3(6) . .
C2 C1 C6 120.5(6) . .
O1 C1 C6 128.2(5) . .
C1 C2 C3 111.3(8) . .
C2 C3 C4 127.9(7) . .
C5 C4 C3 120.9(7) . .
C5 C4 C18 111.7(9) . .
C3 C4 C18 127.3(8) . .
C4 C5 C6 113.0(8) . .
C5 C6 C7 108.9(7) . .
C5 C6 C1 126.4(6) . .
C7 C6 C1 124.6(5) . .
N1 C7 C6 109.1(5) . .
N1 C8 C9 102.3(5) . .
C10 C9 N2 123.1(8) . .
C10 C9 C8 112.6(8) . .
N2 C9 C8 124.2(5) . .
C9 C10 C11 108.9(9) . .
C10 C11 C12 127.7(8) . .
C13 C12 C11 119.4(10) . .
C12 C13 N2 113.9(9) . .
N1 C14 C15 107.9(5) . .
C14 C15 N3 123.7(6) . .
O4 Cl1 O2 118.1(5) . 3_565
O4 Cl1 O2 118.1(5) . .
O2 Cl1 O2 123.7(10) 3_565 .
O4 Cl1 O3 88.3(5) . 3_565
O2 Cl1 O3 80.9(7) 3_565 3_565
O2 Cl1 O3 100.8(7) . 3_565
O4 Cl1 O3 88.3(5) . .
O2 Cl1 O3 100.8(7) 3_565 .
O2 Cl1 O3 80.9(7) . .
O3 Cl1 O3 176.5(11) 3_565 .
C14 N1 C7 110.1(6) . .
C14 N1 C8 107.3(5) . .
C7 N1 C8 102.7(5) . .
C14 N1 Ni1 105.8(5) . .
C7 N1 Ni1 117.8(4) . .
C8 N1 Ni1 112.7(4) . .
C13 N2 C9 126.9(6) . .
C13 N2 Ni1 119.1(5) . .
C9 N2 Ni1 114.0(4) . .
C17 N3 C16 101.2(6) . .
C17 N3 C15 115.3(6) . .
C16 N3 C15 117.2(6) . .
C17 N3 Ni1 113.8(4) . .
C16 N3 Ni1 112.0(4) . .
C15 N3 Ni1 97.9(4) . .
N5 N4 Ni1 125.1(4) . .
N5 N4 Ni1 137.7(4) . 3_566
Ni1 N4 Ni1 96.00(19) . 3_566
N6 N5 N4 179.0(8) . .
O1 Ni1 N3 91.82(18) . .
O1 Ni1 N2 167.4(2) . .
N3 Ni1 N2 96.46(19) . .
O1 Ni1 N4 85.09(17) . .
N3 Ni1 N4 173.6(2) . .
N2 Ni1 N4 87.55(18) . .
O1 Ni1 N1 92.67(17) . .
N3 Ni1 N1 89.85(19) . .
N2 Ni1 N1 77.9(2) . .
N4 Ni1 N1 95.90(18) . .
O1 Ni1 N4 88.75(16) . 3_566
N3 Ni1 N4 91.73(19) . 3_566
N2 Ni1 N4 100.5(2) . 3_566
N4 Ni1 N4 82.61(19) . 3_566
N1 Ni1 N4 177.85(16) . 3_566
C1 O1 Ni1 122.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.341(9) .
C1 O1 1.407(7) .
C1 C6 1.593(10) .
C2 C3 1.458(11) .
C3 C4 1.557(13) .
C4 C5 1.316(11) .
C4 C18 1.580(11) .
C5 C6 1.441(9) .
C6 C7 1.469(9) .
C7 N1 1.465(9) .
C8 N1 1.467(8) .
C8 C9 1.533(10) .
C9 C10 1.354(10) .
C9 N2 1.523(9) .
C10 C11 1.432(16) .
C11 C12 1.567(16) .
C12 C13 1.317(10) .
C13 N2 1.381(9) .
C14 N1 1.360(7) .
C14 C15 1.596(11) .
C15 N3 1.620(10) .
C16 N3 1.564(9) .
C17 N3 1.394(9) .
Cl1 O4 1.275(12) .
Cl1 O2 1.318(7) 3_565
Cl1 O2 1.318(7) .
Cl1 O3 1.620(16) 3_565
Cl1 O3 1.620(16) .
N1 Ni1 2.385(5) .
N2 Ni1 1.995(5) .
N3 Ni1 1.986(4) .
N4 N5 1.254(7) .
N4 Ni1 2.000(4) .
N4 Ni1 2.387(5) 3_566
N5 N6 1.209(8) .
Ni1 O1 1.926(4) .
Ni1 N4 2.387(5) 3_566
