#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/44/7024426.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_7024426
loop_
_publ_author_name
'Wikstrom, Jeffrey P.'
'Filatov, Alexander S.'
'Mikhalyova, Elena A.'
'Shatruk, Michael'
'Foxman, Bruce M.'
'Rybak-Akimova, Elena V'
_publ_section_title
;
 Carbonate formation within a nickel dimer: synthesis of a coordinatively
 unsaturated bis(mu-hydroxo) dinickel complex and its reactivity toward
 carbon dioxide.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2504
_journal_page_last               2514
_journal_paper_doi               10.1039/b916832j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C34 H48 N6 Ni2 O2, 2(Cl O4)'
_chemical_formula_sum            'C34 H48 Cl2 N6 Ni2 O10'
_chemical_formula_weight         889.10
_chemical_name_systematic
;
bis(bis(2-pyridylmethyl)tert-butylamine)
bis(?-methoxo) dinickel perchlorate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                69.725(4)
_cell_angle_beta                 82.290(4)
_cell_angle_gamma                80.908(4)
_cell_formula_units_Z            1
_cell_length_a                   8.356(2)
_cell_length_b                   9.984(3)
_cell_length_c                   12.245(3)
_cell_measurement_reflns_used    7037
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.19
_cell_volume                     942.7(4)
_computing_cell_refinement       'SAINT Ver. 6.22 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8163
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  0.9204
_exptl_absorpt_correction_T_min  0.7527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2003)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0321
_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)+(0.0657P)²+0.5352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                3991
_reflns_number_total             4208
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b916832j.txt
_cod_data_source_block           4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        942.8(4)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7024426
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
Ni1 Ni 0.57525(3) 0.92271(2) 0.617243(18) 0.02085(9) Uani 1 1 d .
Cl1 Cl 0.19941(7) 0.39101(5) 0.81937(5) 0.03581(13) Uani 1 1 d .
O1 O 0.1757(3) 0.4985(2) 0.7078(2) 0.0683(6) Uani 1 1 d .
O2 O 0.0788(3) 0.2956(3) 0.8498(2) 0.0755(7) Uani 1 1 d .
O3 O 0.3589(3) 0.3165(2) 0.8101(3) 0.0781(7) Uani 1 1 d .
O4 O 0.1931(4) 0.4589(3) 0.9036(2) 0.0875(9) Uani 1 1 d .
O5 O 0.63030(15) 1.04561(14) 0.45887(11) 0.0244(3) Uani 1 1 d .
N1 N 0.45895(19) 0.87927(17) 0.78121(14) 0.0251(3) Uani 1 1 d .
N2 N 0.65263(18) 0.69951(15) 0.68491(13) 0.0222(3) Uani 1 1 d .
N3 N 0.77372(19) 0.93914(17) 0.69018(14) 0.0248(3) Uani 1 1 d .
C1 C 0.4105(2) 0.9722(2) 0.84031(18) 0.0307(4) Uani 1 1 d .
H1 H 0.4198 1.0715 0.8015 0.037 Uiso 1 1 calc R
C2 C 0.3478(3) 0.9276(3) 0.95542(19) 0.0370(5) Uani 1 1 d .
H2 H 0.3169 0.9945 0.9960 0.044 Uiso 1 1 calc R
C3 C 0.3308(3) 0.7834(3) 1.01068(18) 0.0402(5) Uani 1 1 d .
H3 H 0.2872 0.7502 1.0898 0.048 Uiso 1 1 calc R
C4 C 0.3777(3) 0.6880(2) 0.94962(18) 0.0344(4) Uani 1 1 d .
H4 H 0.3645 0.5890 0.9856 0.041 Uiso 1 1 calc R
C5 C 0.4443(2) 0.7391(2) 0.83535(16) 0.0250(4) Uani 1 1 d .
C6 C 0.5056(2) 0.64478(19) 0.76146(16) 0.0248(3) Uani 1 1 d .
H6A H 0.5337 0.5444 0.8125 0.030 Uiso 1 1 calc R
H6B H 0.4197 0.6458 0.7127 0.030 Uiso 1 1 calc R
C7 C 0.7034(2) 0.62840(19) 0.59063(17) 0.0264(4) Uani 1 1 d .
C8 C 0.5649(3) 0.6599(2) 0.51192(19) 0.0347(4) Uani 1 1 d .
H8A H 0.5344 0.7641 0.4800 0.052 Uiso 1 1 calc R
H8B H 0.4708 0.6140 0.5576 0.052 Uiso 1 1 calc R
H8C H 0.6009 0.6219 0.4477 0.052 Uiso 1 1 calc R
C9 C 0.7453(3) 0.4650(2) 0.6448(2) 0.0343(4) Uani 1 1 d .
H9A H 0.7861 0.4241 0.5829 0.051 Uiso 1 1 calc R
H9B H 0.6476 0.4223 0.6870 0.051 Uiso 1 1 calc R
H9C H 0.8291 0.4444 0.6992 0.051 Uiso 1 1 calc R
C10 C 0.8511(3) 0.6953(2) 0.5155(2) 0.0381(5) Uani 1 1 d .
H10A H 0.8266 0.8003 0.4875 0.057 Uiso 1 1 calc R
H10B H 0.8765 0.6609 0.4485 0.057 Uiso 1 1 calc R
H10C H 0.9448 0.6674 0.5624 0.057 Uiso 1 1 calc R
C11 C 0.7874(2) 0.67780(19) 0.76103(17) 0.0287(4) Uani 1 1 d .
H11A H 0.8848 0.6262 0.7311 0.034 Uiso 1 1 calc R
H11B H 0.7543 0.6157 0.8410 0.034 Uiso 1 1 calc R
C12 C 0.8329(2) 0.81478(19) 0.76762(15) 0.0240(3) Uani 1 1 d .
C13 C 0.9308(2) 0.8115(2) 0.85164(18) 0.0324(4) Uani 1 1 d .
H13 H 0.9710 0.7226 0.9063 0.039 Uiso 1 1 calc R
C14 C 0.9688(3) 0.9400(3) 0.8545(2) 0.0386(5) Uani 1 1 d .
H14 H 1.0336 0.9403 0.9125 0.046 Uiso 1 1 calc R
C15 C 0.9123(3) 1.0685(2) 0.7724(2) 0.0357(4) Uani 1 1 d .
H15 H 0.9401 1.1575 0.7716 0.043 Uiso 1 1 calc R
C16 C 0.8148(2) 1.0636(2) 0.69234(18) 0.0303(4) Uani 1 1 d .
H16 H 0.7747 1.1512 0.6362 0.036 Uiso 1 1 calc R
C17 C 0.7787(2) 1.1021(2) 0.41073(17) 0.0307(4) Uani 1 1 d .
H17A H 0.7713 1.2003 0.4125 0.046 Uiso 1 1 calc R
H17B H 0.8006 1.1033 0.3298 0.046 Uiso 1 1 calc R
H17C H 0.8672 1.0418 0.4566 0.046 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'
Cl Cl 0.1484 0.1585 '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
O5 Ni1 O5 76.92(6) . 2_676 yes
O5 Ni1 N3 97.86(6) . . yes
O5 Ni1 N3 166.88(6) 2_676 . yes
O5 Ni1 N1 154.28(6) . . yes
O5 Ni1 N1 93.54(6) 2_676 . yes
N3 Ni1 N1 86.12(7) . . yes
O5 Ni1 N2 124.85(6) . . yes
O5 Ni1 N2 109.56(6) 2_676 . yes
N3 Ni1 N2 83.36(6) . . yes
N1 Ni1 N2 80.80(6) . . yes
O4 Cl1 O2 110.59(15) . . ?
O4 Cl1 O1 109.03(17) . . ?
O2 Cl1 O1 110.37(14) . . ?
O4 Cl1 O3 108.79(18) . . ?
O2 Cl1 O3 111.22(16) . . ?
O1 Cl1 O3 106.74(16) . . ?
C17 O5 Ni1 128.24(11) . . ?
C17 O5 Ni1 128.65(11) . 2_676 ?
Ni1 O5 Ni1 103.08(6) . 2_676 ?
C5 N1 C1 119.22(17) . . ?
C5 N1 Ni1 113.38(12) . . ?
C1 N1 Ni1 127.16(14) . . ?
C6 N2 C11 108.34(14) . . ?
C6 N2 C7 112.60(14) . . ?
C11 N2 C7 111.65(14) . . ?
C6 N2 Ni1 101.69(10) . . ?
C11 N2 Ni1 108.16(10) . . ?
C7 N2 Ni1 113.81(11) . . ?
C12 N3 C16 118.90(16) . . ?
C12 N3 Ni1 113.49(12) . . ?
C16 N3 Ni1 124.62(13) . . ?
N1 C1 C2 121.99(19) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 118.74(19) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 121.65(18) . . ?
N1 C5 C6 114.56(16) . . ?
C4 C5 C6 123.79(17) . . ?
N2 C6 C5 109.28(14) . . ?
N2 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N2 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C8 C7 C10 108.21(18) . . ?
C8 C7 C9 109.26(16) . . ?
C10 C7 C9 110.09(16) . . ?
C8 C7 N2 109.52(15) . . ?
C10 C7 N2 108.17(15) . . ?
C9 C7 N2 111.52(15) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 114.39(14) . . ?
N2 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
N2 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N3 C12 C13 121.65(18) . . ?
N3 C12 C11 117.45(16) . . ?
C13 C12 C11 120.90(17) . . ?
C14 C13 C12 118.79(19) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 119.82(19) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 118.17(19) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
N3 C16 C15 122.63(19) . . ?
N3 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
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
Ni1 O5 1.9411(13) . yes
Ni1 O5 1.9932(13) 2_676 yes
Ni1 N3 2.0396(16) . yes
Ni1 N1 2.0421(17) . yes
Ni1 N2 2.1164(15) . yes
Cl1 O4 1.409(2) . ?
Cl1 O2 1.421(2) . ?
Cl1 O1 1.431(2) . ?
Cl1 O3 1.431(2) . ?
O5 C17 1.413(2) . ?
O5 Ni1 1.9932(13) 2_676 yes
N1 C5 1.342(2) . ?
N1 C1 1.348(2) . ?
N2 C6 1.495(2) . ?
N2 C11 1.499(2) . ?
N2 C7 1.536(2) . ?
N3 C12 1.342(2) . ?
N3 C16 1.350(2) . ?
C1 C2 1.379(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.383(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.511(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.530(3) . ?
C7 C10 1.532(3) . ?
C7 C9 1.535(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.507(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.387(3) . ?
C13 C14 1.382(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
