#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:57:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179401 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/98/4329818.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_4329818
loop_
_publ_author_name
'Rituparna Biswas'
'Sandip Mukherjee'
'Paramita Kar'
'Ashutosh Ghosh'
_publ_section_title
;
 A Rare Phenoxido/Acetato/Azido Bridged Trinuclear and an Unprecedented
 Phenoxido/Azido Bridged One-Dimensional Polynuclear Nickel(II) Complexes:
 Synthesis, Crystal Structure, and Magnetic Properties with Theoretical
 Investigations on the Exchange Mechanism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8150
_journal_page_last               8160
_journal_paper_doi               10.1021/ic300547w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C12 H17 N5 Ni O'
_chemical_formula_weight         306.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b 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            8
_cell_length_a                   17.8499(18)
_cell_length_b                   13.2590(13)
_cell_length_c                   11.9339(12)
_cell_measurement_temperature    293(2)
_cell_volume                     2824.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1997)'
_computing_publication_material  'Platon99 (Spek, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33083
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.8975
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0370
_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)+(0.0383P)²+1.7178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                2214
_reflns_number_total             3106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300547w_si_001_2.cif
_cod_data_source_block           2
_cod_database_code               4329818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, 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
Ni1 Ni 0.064220(17) 0.10950(2) 0.17858(3) 0.03936(13) Uani 1 1 d .
O1 O 0.05055(9) 0.16509(14) 0.33377(14) 0.0437(4) Uani 1 1 d .
N1 N 0.17611(12) 0.05175(18) 0.1974(2) 0.0538(6) Uani 1 1 d .
N4 N 0.0000 0.0000 0.0000 0.0492(8) Uani 1 2 d S
N3 N 0.05562(13) 0.0423(2) 0.0229(2) 0.0600(7) Uani 1 1 d .
N2 N 0.11390(11) 0.23798(17) 0.12877(19) 0.0459(5) Uani 1 1 d .
N007 N 0.0000 -0.0960(3) 0.2500 0.0554(9) Uani 1 2 d S
N5 N 0.0000 -0.0058(2) 0.2500 0.0493(8) Uani 1 2 d S
C12 C 0.06380(13) 0.2572(2) 0.3692(2) 0.0471(6) Uani 1 1 d .
C7 C 0.09135(14) 0.3345(2) 0.2990(3) 0.0504(7) Uani 1 1 d .
C6 C 0.11687(14) 0.3191(2) 0.1867(3) 0.0510(7) Uani 1 1 d .
H6 H 0.1382 0.3748 0.1516 0.061 Uiso 1 1 calc R
C11 C 0.05058(16) 0.2805(3) 0.4828(3) 0.0631(8) Uani 1 1 d .
H11 H 0.0347 0.2301 0.5315 0.076 Uiso 1 1 calc R
C4 C 0.23022(17) 0.1745(3) 0.0527(3) 0.0691(9) Uani 1 1 d .
H4A H 0.2609 0.1733 -0.0143 0.083 Uiso 1 1 calc R
H4B H 0.2577 0.2116 0.1094 0.083 Uiso 1 1 calc R
C9 C 0.08536(19) 0.4526(3) 0.4538(4) 0.0882(13) Uani 1 1 d .
H9 H 0.0919 0.5175 0.4818 0.106 Uiso 1 1 calc R
C5 C 0.15867(16) 0.2323(2) 0.0265(3) 0.0612(8) Uani 1 1 d .
H5A H 0.1708 0.2997 0.0004 0.073 Uiso 1 1 calc R
H5B H 0.1307 0.1980 -0.0319 0.073 Uiso 1 1 calc R
C8 C 0.10003(17) 0.4324(3) 0.3445(4) 0.0711(10) Uani 1 1 d .
H8 H 0.1162 0.4844 0.2981 0.085 Uiso 1 1 calc R
C10 C 0.06095(18) 0.3768(3) 0.5225(4) 0.0810(12) Uani 1 1 d .
H10 H 0.0512 0.3907 0.5974 0.097 Uiso 1 1 calc R
C3 C 0.22045(17) 0.0667(3) 0.0934(3) 0.0677(9) Uani 1 1 d .
H3A H 0.1968 0.0283 0.0340 0.081 Uiso 1 1 calc R
H3B H 0.2698 0.0381 0.1053 0.081 Uiso 1 1 calc R
N6 N 0.0000 -0.1825(3) 0.2500 0.0949(16) Uani 1 2 d S
C1 C 0.21280(18) 0.1001(3) 0.2949(3) 0.0715(10) Uani 1 1 d .
H1A H 0.2164 0.1715 0.2824 0.107 Uiso 1 1 calc R
H1B H 0.2621 0.0725 0.3044 0.107 Uiso 1 1 calc R
H1C H 0.1837 0.0876 0.3612 0.107 Uiso 1 1 calc R
C2 C 0.17183(19) -0.0580(3) 0.2187(4) 0.0822(11) Uani 1 1 d .
H2A H 0.1434 -0.0700 0.2856 0.123 Uiso 1 1 calc R
H2B H 0.2215 -0.0846 0.2278 0.123 Uiso 1 1 calc R
H2C H 0.1479 -0.0906 0.1565 0.123 Uiso 1 1 calc R
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'
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
O1 Ni1 N2 90.88(8) . .
O1 Ni1 N3 168.10(8) . .
N2 Ni1 N3 97.60(10) . .
O1 Ni1 N5 79.97(7) . .
N2 Ni1 N5 168.88(9) . .
N3 Ni1 N5 90.61(8) . .
O1 Ni1 N1 98.45(8) . .
N2 Ni1 N1 85.58(9) . .
N3 Ni1 N1 90.55(10) . .
N5 Ni1 N1 101.90(8) . .
O1 Ni1 O1 79.87(8) . 4
N2 Ni1 O1 96.20(8) . 4
N3 Ni1 O1 90.87(9) . 4
N5 Ni1 O1 76.10(6) . 4
N1 Ni1 O1 177.56(8) . 4
O1 Ni1 Ni1 49.62(5) . 4
N2 Ni1 Ni1 122.03(6) . 4
N3 Ni1 Ni1 118.48(7) . 4
N5 Ni1 Ni1 46.93(6) . 4
N1 Ni1 Ni1 133.06(7) . 4
O1 Ni1 Ni1 44.51(5) 4 4
C12 O1 Ni1 128.02(18) . .
C12 O1 Ni1 120.32(15) . 4
Ni1 O1 Ni1 85.86(6) . 4
C2 N1 C1 108.3(3) . .
C2 N1 C3 107.6(2) . .
C1 N1 C3 111.3(3) . .
C2 N1 Ni1 108.67(19) . .
C1 N1 Ni1 109.80(17) . .
C3 N1 Ni1 111.10(19) . .
N3 N4 N3 180.0(3) 5 .
N4 N3 Ni1 118.59(16) . .
C6 N2 C5 118.2(2) . .
C6 N2 Ni1 124.80(19) . .
C5 N2 Ni1 116.41(19) . .
N6 N007 N5 180.0 . .
N007 N5 Ni1 136.93(6) . .
N007 N5 Ni1 136.93(6) . 4
Ni1 N5 Ni1 86.13(12) . 4
O1 C12 C11 118.9(3) . .
O1 C12 C7 123.1(2) . .
C11 C12 C7 118.0(3) . .
C12 C7 C8 118.4(3) . .
C12 C7 C6 124.3(3) . .
C8 C7 C6 117.1(3) . .
N2 C6 C7 127.8(3) . .
C10 C11 C12 120.8(4) . .
C3 C4 C5 116.3(2) . .
C8 C9 C10 119.5(3) . .
N2 C5 C4 108.2(2) . .
C9 C8 C7 121.9(4) . .
C9 C10 C11 121.2(4) . .
N1 C3 C4 117.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0081(17) .
Ni1 N2 2.010(2) .
Ni1 N3 2.066(2) .
Ni1 N5 2.092(2) .
Ni1 N1 2.151(2) .
Ni1 O1 2.1821(17) 4
Ni1 Ni1 2.8569(6) 4
O1 C12 1.314(3) .
O1 Ni1 2.1821(17) 4
N1 C2 1.479(4) .
N1 C1 1.481(4) .
N1 C3 1.485(4) .
N4 N3 1.173(2) 5
N4 N3 1.173(2) .
N2 C6 1.280(3) .
N2 C5 1.461(4) .
N007 N6 1.147(5) .
N007 N5 1.197(4) .
N5 Ni1 2.092(2) 4
C12 C11 1.411(4) .
C12 C7 1.412(4) .
C7 C8 1.416(4) .
C7 C6 1.430(4) .
C11 C10 1.374(5) .
C4 C3 1.520(5) .
C4 C5 1.522(4) .
C9 C8 1.357(6) .
C9 C10 1.368(6) .
