#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004613.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_7004613
loop_
_publ_author_name
'Banerjee, Atanu'
'Singh, Reena'
'Chopra, Deepak'
'Colacio, Enrique'
'Rajak, Kajal Krishna'
_publ_section_title
;
 Mixed bridged dinuclear Ni(II) complexes: synthesis, structure,
 magnetic properties and DFT study
;
_journal_issue                   46
_journal_name_full               'Dalton Transactions'
_journal_page_first              6539
_journal_page_last               6545
_journal_paper_doi               10.1039/b809197h
_journal_year                    2008
_chemical_formula_sum            'C32 H49 N7 Ni2 O6'
_chemical_formula_weight         745.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.438(2)
_cell_angle_beta                 99.001(2)
_cell_angle_gamma                114.755(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4736(13)
_cell_length_b                   11.0275(13)
_cell_length_c                   17.238(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.04
_cell_volume                     1776.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18586
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (SADABAS,SHELDRICK-1997)
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallopiped
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0494
_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)+(0.0673P)²+1.1274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                5327
_reflns_number_total             6943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809197h.txt
_cod_data_source_block           '[Ni2(L)(N3)(H2O)].H2O.CH3OH'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7004613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1870(3) 0.6442(3) 0.17583(19) 0.0325(7) Uani 1 1 d . . .
C2 C -0.0691(4) 0.6248(3) 0.1592(2) 0.0374(8) Uani 1 1 d . . .
C3 C -0.0911(4) 0.5193(3) 0.1054(2) 0.0425(8) Uani 1 1 d . . .
H3A H -0.0121 0.5085 0.0945 0.051 Uiso 1 1 calc R . .
C4 C -0.2261(4) 0.4294(3) 0.0674(2) 0.0457(9) Uani 1 1 d . . .
C5 C -0.3412(4) 0.4507(3) 0.0837(2) 0.0432(9) Uani 1 1 d . . .
H5A H -0.4330 0.3916 0.0589 0.052 Uiso 1 1 calc R . .
C6 C -0.3250(4) 0.5563(3) 0.13550(19) 0.0363(8) Uani 1 1 d . . .
C7 C 0.0803(4) 0.7165(3) 0.2006(2) 0.0405(8) Uani 1 1 d . . .
H7A H 0.0901 0.6994 0.2556 0.049 Uiso 1 1 calc R . .
H7B H 0.1474 0.6938 0.1777 0.049 Uiso 1 1 calc R . .
C8 C 0.0920(4) 0.8897(4) 0.1129(2) 0.0417(8) Uani 1 1 d . . .
H8A H -0.0068 0.8309 0.0903 0.050 Uiso 1 1 calc R . .
H8B H 0.1520 0.8664 0.0837 0.050 Uiso 1 1 calc R . .
C9 C 0.1167(4) 1.0319(4) 0.1008(2) 0.0399(8) Uani 1 1 d . . .
C10 C 0.0381(4) 1.0885(4) 0.1349(2) 0.0403(8) Uani 1 1 d . . .
C11 C 0.0556(4) 1.2178(4) 0.1165(2) 0.0513(10) Uani 1 1 d . . .
H11A H 0.0042 1.2572 0.1379 0.062 Uiso 1 1 calc R . .
C12 C 0.1471(5) 1.2864(4) 0.0675(2) 0.0590(12) Uani 1 1 d . . .
H12A H 0.1569 1.3716 0.0563 0.071 Uiso 1 1 calc R . .
C13 C 0.2238(4) 1.2317(4) 0.0350(2) 0.0606(12) Uani 1 1 d . . .
H13A H 0.2858 1.2792 0.0020 0.073 Uiso 1 1 calc R . .
C14 C 0.2084(4) 1.1042(4) 0.0517(2) 0.0518(10) Uani 1 1 d . . .
H14A H 0.2607 1.0667 0.0294 0.062 Uiso 1 1 calc R . .
C15 C 0.2752(4) 0.9394(4) 0.2335(2) 0.0476(9) Uani 1 1 d . . .
H15A H 0.3337 0.9504 0.1935 0.057 Uiso 1 1 calc R . .
H15B H 0.3017 0.8893 0.2734 0.057 Uiso 1 1 calc R . .
C16 C 0.3035(4) 1.0758(4) 0.2709(2) 0.0452(9) Uani 1 1 d . . .
H16A H 0.3998 1.1179 0.3016 0.054 Uiso 1 1 calc R . .
H16B H 0.2961 1.1325 0.2300 0.054 Uiso 1 1 calc R . .
C17 C -0.4539(4) 0.5786(4) 0.1445(2) 0.0403(8) Uani 1 1 d . . .
H17A H -0.4455 0.6605 0.1217 0.048 Uiso 1 1 calc R . .
H17B H -0.5379 0.5053 0.1140 0.048 Uiso 1 1 calc R . .
C18 C -0.6152(4) 0.6025(4) 0.2216(2) 0.0439(9) Uani 1 1 d . . .
H18A H -0.6063 0.6810 0.1947 0.053 Uiso 1 1 calc R . .
H18B H -0.6907 0.5248 0.1893 0.053 Uiso 1 1 calc R . .
C19 C -0.6591(4) 0.6149(4) 0.2986(2) 0.0432(9) Uani 1 1 d . . .
C20 C -0.5713(4) 0.7263(4) 0.3545(2) 0.0434(9) Uani 1 1 d . . .
C21 C -0.6224(4) 0.7411(4) 0.4231(2) 0.0541(10) Uani 1 1 d . . .
H21A H -0.5669 0.8139 0.4606 0.065 Uiso 1 1 calc R . .
C22 C -0.7546(5) 0.6486(5) 0.4359(3) 0.0662(13) Uani 1 1 d . . .
H22A H -0.7870 0.6603 0.4815 0.079 Uiso 1 1 calc R . .
C23 C -0.8384(5) 0.5391(5) 0.3810(3) 0.0634(12) Uani 1 1 d . . .
H23A H -0.9264 0.4766 0.3898 0.076 Uiso 1 1 calc R . .
C24 C -0.7904(4) 0.5237(4) 0.3134(3) 0.0520(10) Uani 1 1 d . . .
H24A H -0.8471 0.4503 0.2766 0.062 Uiso 1 1 calc R . .
C25 C -0.4828(4) 0.4703(3) 0.2670(2) 0.0425(8) Uani 1 1 d . . .
H25A H -0.4237 0.4351 0.2452 0.051 Uiso 1 1 calc R . .
H25B H -0.5803 0.4010 0.2567 0.051 Uiso 1 1 calc R . .
C26 C -0.4311(4) 0.5040(4) 0.3552(3) 0.0586(11) Uani 1 1 d . . .
H26A H -0.5026 0.5183 0.3787 0.070 Uiso 1 1 calc R . .
H26B H -0.4195 0.4286 0.3777 0.070 Uiso 1 1 calc R . .
C27 C 0.1996(4) 1.1952(4) 0.3390(2) 0.0523(10) Uani 1 1 d . . .
H27A H 0.2921 1.2565 0.3675 0.078 Uiso 1 1 calc R . .
H27B H 0.1283 1.1865 0.3701 0.078 Uiso 1 1 calc R . .
H27C H 0.1791 1.2287 0.2900 0.078 Uiso 1 1 calc R . .
C28 C 0.2350(5) 1.0129(5) 0.3989(2) 0.0631(12) Uani 1 1 d . . .
H28A H 0.3250 1.0783 0.4277 0.095 Uiso 1 1 calc R . .
H28B H 0.2415 0.9299 0.3887 0.095 Uiso 1 1 calc R . .
H28C H 0.1617 0.9987 0.4296 0.095 Uiso 1 1 calc R . .
C29 C -0.1701(5) 0.5958(5) 0.3738(3) 0.0727(14) Uani 1 1 d . . .
H29A H -0.1678 0.5353 0.4125 0.109 Uiso 1 1 calc R . .
H29B H -0.0842 0.6779 0.3859 0.109 Uiso 1 1 calc R . .
H29C H -0.1769 0.5555 0.3224 0.109 Uiso 1 1 calc R . .
C30 C -0.2814(6) 0.6804(5) 0.4563(3) 0.0760(14) Uani 1 1 d . . .
H30A H -0.2731 0.6187 0.4928 0.114 Uiso 1 1 calc R . .
H30B H -0.3648 0.6944 0.4603 0.114 Uiso 1 1 calc R . .
H30C H -0.1979 0.7645 0.4685 0.114 Uiso 1 1 calc R . .
C31 C -0.2481(5) 0.3134(4) 0.0097(3) 0.0700(13) Uani 1 1 d . . .
H31A H -0.1571 0.3147 0.0058 0.105 Uiso 1 1 calc R . .
H31B H -0.2943 0.3216 -0.0412 0.105 Uiso 1 1 calc R . .
H31C H -0.3069 0.2303 0.0281 0.105 Uiso 1 1 calc R . .
C32 C -0.2245(11) 1.2356(8) 0.2493(6) 0.181(4) Uani 1 1 d . . .
H32A H -0.2429 1.2958 0.2148 0.272 Uiso 1 1 calc R . .
H32B H -0.1614 1.2049 0.2293 0.272 Uiso 1 1 calc R . .
H32C H -0.1807 1.2816 0.3012 0.272 Uiso 1 1 calc R . .
N1 N 0.1213(3) 0.8627(3) 0.19688(17) 0.0357(6) Uani 1 1 d . . .
N2 N 0.1988(3) 1.0621(3) 0.32281(17) 0.0410(7) Uani 1 1 d . . .
N3 N -0.4776(3) 0.5886(3) 0.22734(16) 0.0342(6) Uani 1 1 d . . .
N4 N -0.2944(3) 0.6245(3) 0.37469(17) 0.0409(7) Uani 1 1 d . . .
N5 N -0.1196(3) 0.9256(3) 0.3469(2) 0.0411(7) Uani 1 1 d . . .
N6 N -0.1065(3) 1.0050(4) 0.3898(2) 0.0567(9) Uani 1 1 d . . .
N7 N -0.0909(5) 1.0923(5) 0.4392(3) 0.0932(16) Uani 1 1 d . . .
O1 O -0.0484(3) 1.0249(2) 0.18401(15) 0.0441(6) Uani 1 1 d . . .
O2 O -0.1686(2) 0.7424(2) 0.22935(14) 0.0359(5) Uani 1 1 d . . .
O3 O -0.4437(3) 0.8128(2) 0.34349(16) 0.0484(6) Uani 1 1 d . . .
O4 O -0.3325(3) 0.8888(3) 0.19904(16) 0.0521(7) Uani 1 1 d . . .
H4A H -0.3402 0.8622 0.1480 0.063 Uiso 1 1 d R . .
H4B H -0.3329 0.9680 0.2124 0.063 Uiso 1 1 d R . .
O5 O -0.3603(6) 1.1196(6) 0.2532(4) 0.160(2) Uani 1 1 d . . .
H5B H -0.4350 1.1345 0.2210 0.192 Uiso 1 1 d R . .
O6 O -0.3892(4) 1.0639(4) 0.3959(3) 0.1126(14) Uani 1 1 d . . .
H6A H -0.3194 1.1131 0.4366 0.135 Uiso 1 1 d R . .
H6B H -0.4686 0.9950 0.4050 0.135 Uiso 1 1 d R . .
Ni1 Ni 0.00216(4) 0.91923(4) 0.26143(2) 0.03223(14) Uani 1 1 d . . .
Ni2 Ni -0.31346(4) 0.76051(4) 0.28988(2) 0.03386(14) Uani 1 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'
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
_geom_angle_publ_flag
O2 C1 C2 120.6(3) . . ?
O2 C1 C6 120.8(3) . . ?
C2 C1 C6 118.5(3) . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 C7 119.9(3) . . ?
C1 C2 C7 120.4(3) . . ?
C4 C3 C2 122.6(3) . . ?
C3 C4 C5 117.1(3) . . ?
C3 C4 C31 121.8(4) . . ?
C5 C4 C31 121.2(4) . . ?
C6 C5 C4 122.7(3) . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C17 119.1(3) . . ?
C1 C6 C17 121.4(3) . . ?
N1 C7 C2 115.2(3) . . ?
N1 C8 C9 115.4(3) . . ?
C14 C9 C10 119.6(3) . . ?
C14 C9 C8 120.6(3) . . ?
C10 C9 C8 119.6(3) . . ?
O1 C10 C9 122.0(3) . . ?
O1 C10 C11 120.2(4) . . ?
C9 C10 C11 117.7(3) . . ?
C12 C11 C10 121.1(4) . . ?
C13 C12 C11 121.1(4) . . ?
C12 C13 C14 119.3(4) . . ?
C9 C14 C13 121.2(4) . . ?
N1 C15 C16 111.0(3) . . ?
N2 C16 C15 110.1(3) . . ?
N3 C17 C6 115.6(3) . . ?
C19 C18 N3 115.2(3) . . ?
C24 C19 C20 119.7(4) . . ?
C24 C19 C18 120.6(4) . . ?
C20 C19 C18 119.6(3) . . ?
O3 C20 C21 120.8(4) . . ?
O3 C20 C19 121.3(3) . . ?
C21 C20 C19 117.9(4) . . ?
C22 C21 C20 121.0(4) . . ?
C23 C22 C21 120.3(4) . . ?
C24 C23 C22 119.4(4) . . ?
C23 C24 C19 121.7(4) . . ?
N3 C25 C26 111.8(3) . . ?
N4 C26 C25 112.0(3) . . ?
C7 N1 C15 109.0(3) . . ?
C7 N1 C8 109.6(3) . . ?
C15 N1 C8 111.8(3) . . ?
C7 N1 Ni1 109.0(2) . . ?
C15 N1 Ni1 108.0(2) . . ?
C8 N1 Ni1 109.3(2) . . ?
C27 N2 C16 108.8(3) . . ?
C27 N2 C28 109.0(3) . . ?
C16 N2 C28 111.4(3) . . ?
C27 N2 Ni1 113.1(2) . . ?
C16 N2 Ni1 105.6(2) . . ?
C28 N2 Ni1 109.0(2) . . ?
C25 N3 C17 111.1(3) . . ?
C25 N3 C18 111.9(3) . . ?
C17 N3 C18 106.3(3) . . ?
C25 N3 Ni2 109.5(2) . . ?
C17 N3 Ni2 109.3(2) . . ?
C18 N3 Ni2 108.6(2) . . ?
C29 N4 C26 113.0(3) . . ?
C29 N4 C30 106.9(3) . . ?
C26 N4 C30 107.8(3) . . ?
C29 N4 Ni2 113.6(2) . . ?
C26 N4 Ni2 104.6(2) . . ?
C30 N4 Ni2 110.9(3) . . ?
N6 N5 Ni1 131.8(3) . . ?
N6 N5 Ni2 128.4(3) . . ?
Ni1 N5 Ni2 95.61(13) . . ?
N5 N6 N7 178.4(5) . . ?
C10 O1 Ni1 121.4(2) . . ?
C1 O2 Ni1 128.44(19) . . ?
C1 O2 Ni2 128.94(19) . . ?
Ni1 O2 Ni2 102.31(10) . . ?
C20 O3 Ni2 123.6(2) . . ?
O1 Ni1 O2 99.06(10) . . ?
O1 Ni1 N1 96.74(11) . . ?
O2 Ni1 N1 91.59(10) . . ?
O1 Ni1 N2 101.10(11) . . ?
O2 Ni1 N2 159.83(11) . . ?
N1 Ni1 N2 85.51(11) . . ?
O1 Ni1 N5 100.57(11) . . ?
O2 Ni1 N5 80.28(10) . . ?
N1 Ni1 N5 161.82(11) . . ?
N2 Ni1 N5 96.51(11) . . ?
O3 Ni2 O2 169.46(10) . . ?
O3 Ni2 N3 94.57(10) . . ?
O2 Ni2 N3 91.69(10) . . ?
O3 Ni2 N5 95.34(11) . . ?
O2 Ni2 N5 78.72(11) . . ?
N3 Ni2 N5 170.00(11) . . ?
O3 Ni2 N4 95.18(11) . . ?
O2 Ni2 N4 93.89(10) . . ?
N3 Ni2 N4 84.16(11) . . ?
N5 Ni2 N4 93.60(11) . . ?
O3 Ni2 O4 87.63(11) . . ?
O2 Ni2 O4 83.51(10) . . ?
N3 Ni2 O4 93.56(10) . . ?
N5 Ni2 O4 88.20(11) . . ?
N4 Ni2 O4 176.51(11) . . ?
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
C1 O2 1.335(4) . ?
C1 C2 1.408(5) . ?
C1 C6 1.411(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.507(5) . ?
C3 C4 1.384(5) . ?
C4 C5 1.389(5) . ?
C4 C31 1.515(5) . ?
C5 C6 1.384(5) . ?
C6 C17 1.500(5) . ?
C7 N1 1.490(4) . ?
C8 N1 1.496(4) . ?
C8 C9 1.504(5) . ?
C9 C14 1.387(5) . ?
C9 C10 1.405(5) . ?
C10 O1 1.329(4) . ?
C10 C11 1.411(5) . ?
C11 C12 1.371(6) . ?
C12 C13 1.361(6) . ?
C13 C14 1.389(6) . ?
C15 N1 1.492(4) . ?
C15 C16 1.511(5) . ?
C16 N2 1.484(4) . ?
C17 N3 1.496(4) . ?
C18 C19 1.493(5) . ?
C18 N3 1.500(4) . ?
C19 C24 1.390(5) . ?
C19 C20 1.414(5) . ?
C20 O3 1.324(4) . ?
C20 C21 1.405(5) . ?
C21 C22 1.388(6) . ?
C22 C23 1.386(7) . ?
C23 C24 1.371(6) . ?
C25 N3 1.473(4) . ?
C25 C26 1.514(5) . ?
C26 N4 1.471(5) . ?
C27 N2 1.484(5) . ?
C28 N2 1.487(5) . ?
C29 N4 1.465(5) . ?
C30 N4 1.484(5) . ?
C32 O5 1.475(8) . ?
N1 Ni1 2.058(3) . ?
N2 Ni1 2.088(3) . ?
N3 Ni2 2.073(3) . ?
N4 Ni2 2.167(3) . ?
N5 N6 1.080(4) . ?
N5 Ni1 2.111(3) . ?
N5 Ni2 2.143(3) . ?
N6 N7 1.210(5) . ?
O1 Ni1 1.948(2) . ?
O2 Ni1 2.005(2) . ?
O2 Ni2 2.042(2) . ?
O3 Ni2 2.018(2) . ?
O4 Ni2 2.178(3) . ?
