#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:30:28 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179183 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/30/4313043.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_4313043
loop_
_publ_author_name
'Michael J. Goldcamp'
'Sara E. Edison'
'Leah N. Squires'
'Dell T. Rosa'
'Neil K. Vowels'
'Nathan L. Coker'
'Jeanette A. Krause Bauer'
'Michael J. Baldwin'
_publ_contact_author_address
;     Department of Chemistry
      University of Cincinnati
      Cincinnati, OH 45221-0172 USA
;
_publ_contact_author_email       jeanette.krause@uc.edu
_publ_contact_author_fax         '513 556 9239'
_publ_contact_author_name        'Dr. Jeanette A. Krause Bauer'
_publ_contact_author_phone       '513 556 9226'
_publ_section_title
;
 Structural and Spectroscopic Studies of Nickel(II) Complexes with a
 Library of Bis(oxime)amine-Containing Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              717
_journal_page_last               728
_journal_paper_doi               10.1021/ic025860q
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C28 H42 Cl4 N6 Ni2 O4'
_chemical_formula_weight         785.90
_chemical_name_common            '[Ni(PEABOH₂)Cl]₂(μ-Cl)₂'
_chemical_name_systematic
; 
 Nickel(II) (N-phenethyl-N,N-bis(1-propan-2-onyl oxime)amine) 
chloride 
;
_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   mixed
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.4070(10)
_cell_angle_beta                 100.9850(10)
_cell_angle_gamma                94.5750(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4695(2)
_cell_length_b                   10.2688(3)
_cell_length_c                   10.5412(2)
_cell_measurement_reflns_used    5688
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.87
_cell_volume                     826.64(4)
_computing_cell_refinement       'SMART v5.054'
_computing_data_collection       'SMART v5.054'
_computing_data_reduction        'SAINT v5.A06'
_computing_molecular_graphics    'SHELXTL v5.1'
_computing_publication_material  'SHELXTL v5.1'
_computing_structure_refinement  'SHELXTL v5.1'
_computing_structure_solution    'SHELXTL v5.1'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SMART 1K Platform CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8658
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    1.506
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,1996'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0342P)²+0.0247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                3448
_reflns_number_total             3978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025860q_s2_04.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        826.64(3)
_cod_database_code               4313043
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
Ni Ni 0.52041(2) -0.053987(19) 0.644538(19) 0.01409(6) Uani 1 1 d . . .
Cl1 Cl 0.80537(4) 0.05339(4) 0.76157(4) 0.02105(9) Uani 1 1 d . . .
Cl2 Cl 0.56411(4) -0.14117(4) 0.41272(4) 0.01791(8) Uani 1 1 d . . .
O1 O 0.73989(13) -0.26393(12) 0.67848(13) 0.0265(3) Uani 1 1 d . . .
H1 H 0.7955 -0.1823 0.6834 0.040 Uiso 1 1 d . . .
O2 O 0.56461(13) 0.13607(12) 0.95457(11) 0.0231(2) Uani 1 1 d . . .
H2 H 0.6526 0.1367 0.9200 0.035 Uiso 1 1 d . . .
N1 N 0.58129(14) -0.23285(13) 0.67022(13) 0.0173(3) Uani 1 1 d . . .
N2 N 0.45655(14) 0.03911(13) 0.83241(13) 0.0168(2) Uani 1 1 d . . .
N3 N 0.27986(14) -0.17578(13) 0.61415(13) 0.0166(2) Uani 1 1 d . . .
C1 C 0.30875(18) -0.28685(16) 0.67222(17) 0.0206(3) Uani 1 1 d . . .
H1A H 0.2281 -0.3735 0.6140 0.025 Uiso 1 1 calc R . .
H1B H 0.2908 -0.2529 0.7683 0.025 Uiso 1 1 calc R . .
C2 C 0.47738(18) -0.32387(16) 0.67710(15) 0.0184(3) Uani 1 1 d . . .
C3 C 0.5080(2) -0.45695(17) 0.6973(2) 0.0291(4) Uani 1 1 d . . .
H3A H 0.4506 -0.4680 0.7661 0.044 Uiso 1 1 calc R . .
H3B H 0.6252 -0.4519 0.7314 0.044 Uiso 1 1 calc R . .
H3C H 0.4682 -0.5383 0.6078 0.044 Uiso 1 1 calc R . .
C4 C 0.19289(17) -0.07196(16) 0.70208(16) 0.0199(3) Uani 1 1 d . . .
H4A H 0.1038 -0.1233 0.7230 0.024 Uiso 1 1 calc R . .
H4B H 0.1436 -0.0167 0.6497 0.024 Uiso 1 1 calc R . .
C5 C 0.30668(18) 0.02729(16) 0.83701(16) 0.0182(3) Uani 1 1 d . . .
C6 C 0.2392(2) 0.10537(18) 0.95877(17) 0.0244(3) Uani 1 1 d . . .
H6A H 0.2123 0.0419 1.0048 0.037 Uiso 1 1 calc R . .
H6B H 0.1404 0.1389 0.9260 0.037 Uiso 1 1 calc R . .
H6C H 0.3203 0.1866 1.0257 0.037 Uiso 1 1 calc R . .
C7 C 0.18784(17) -0.24128(16) 0.46469(16) 0.0189(3) Uani 1 1 d . . .
H7A H 0.2451 -0.3162 0.4128 0.023 Uiso 1 1 calc R . .
H7B H 0.1897 -0.1680 0.4244 0.023 Uiso 1 1 calc R . .
C8 C 0.00851(18) -0.30698(17) 0.44014(17) 0.0228(3) Uani 1 1 d . . .
H8A H 0.0025 -0.3630 0.4986 0.027 Uiso 1 1 calc R . .
H8B H -0.0568 -0.2302 0.4694 0.027 Uiso 1 1 calc R . .
C9 C -0.06267(17) -0.40161(16) 0.28784(16) 0.0195(3) Uani 1 1 d . . .
C10 C -0.00883(19) -0.53000(17) 0.22666(19) 0.0257(3) Uani 1 1 d . . .
H10 H 0.0744 -0.5577 0.2810 0.031 Uiso 1 1 calc R . .
C11 C -0.0757(2) -0.61770(18) 0.0871(2) 0.0313(4) Uani 1 1 d . . .
H11 H -0.0375 -0.7045 0.0468 0.038 Uiso 1 1 calc R . .
C12 C -0.1975(2) -0.57973(19) 0.00636(19) 0.0330(4) Uani 1 1 d . . .
H12 H -0.2427 -0.6396 -0.0892 0.040 Uiso 1 1 calc R . .
C13 C -0.2527(2) -0.4531(2) 0.06674(19) 0.0308(4) Uani 1 1 d . . .
H13 H -0.3374 -0.4266 0.0126 0.037 Uiso 1 1 calc R . .
C14 C -0.18505(19) -0.36486(17) 0.20579(17) 0.0238(3) Uani 1 1 d . . .
H14 H -0.2232 -0.2778 0.2454 0.029 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
N1 Ni N2 97.53(5) . . y
N1 Ni N3 77.73(5) . . y
N2 Ni N3 75.66(5) . . y
N1 Ni Cl2 90.75(4) . . y
N2 Ni Cl2 170.68(3) . . y
N3 Ni Cl2 102.11(3) . . y
N1 Ni Cl2 173.69(4) . 2_656 y
N2 Ni Cl2 87.48(3) . 2_656 y
N3 Ni Cl2 99.93(3) . 2_656 y
Cl2 Ni Cl2 83.988(13) . 2_656 y
N1 Ni Cl1 86.18(4) . . y
N2 Ni Cl1 89.50(4) . . y
N3 Ni Cl1 156.28(3) . . y
Cl2 Ni Cl1 95.343(14) . . y
Cl2 Ni Cl1 97.750(14) 2_656 . y
Ni Cl2 Ni 96.012(13) . 2_656 y
C2 N1 O1 115.67(12) . . y
C2 N1 Ni 122.10(10) . . y
O1 N1 Ni 122.23(9) . . y
C5 N2 O2 115.46(12) . . y
C5 N2 Ni 119.96(10) . . y
O2 N2 Ni 123.72(8) . . y
C4 N3 C7 111.77(11) . . y
C4 N3 C1 109.12(11) . . y
C7 N3 C1 110.71(12) . . y
C4 N3 Ni 104.73(9) . . y
C7 N3 Ni 113.11(9) . . y
C1 N3 Ni 107.10(8) . . y
N3 C1 C2 113.32(12) . . y
N1 C2 C3 126.78(14) . . y
N1 C2 C1 114.97(13) . . y
C3 C2 C1 118.15(13) . . y
N3 C4 C5 111.16(12) . . y
N2 C5 C6 126.24(14) . . y
N2 C5 C4 114.19(13) . . y
C6 C5 C4 119.53(13) . . y
N3 C7 C8 115.09(12) . . y
C9 C8 C7 111.47(12) . . y
C14 C9 C10 118.19(15) . . y
C14 C9 C8 121.09(14) . . y
C10 C9 C8 120.71(14) . . y
C11 C10 C9 120.66(16) . . y
C12 C11 C10 120.59(16) . . y
C11 C12 C13 119.09(17) . . y
C12 C13 C14 120.37(17) . . y
C9 C14 C13 121.09(15) . . y
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
Ni N1 2.0429(12) . y
Ni N2 2.0584(12) . y
Ni N3 2.2068(12) . y
Ni Cl2 2.3897(4) . y
Ni Cl2 2.4166(4) 2_656 y
Ni Cl1 2.4515(4) . y
O1 N1 1.3993(15) . y
O2 N2 1.3988(15) . y
N1 C2 1.2633(19) . y
N2 C5 1.2773(18) . y
N3 C4 1.4840(18) . y
N3 C7 1.4889(19) . y
N3 C1 1.4942(18) . y
C1 C2 1.503(2) . y
C2 C3 1.493(2) . y
C4 C5 1.501(2) . y
C5 C6 1.490(2) . y
C7 C8 1.545(2) . y
C8 C9 1.511(2) . y
C9 C14 1.387(2) . y
C9 C10 1.396(2) . y
C10 C11 1.389(2) . y
C11 C12 1.382(3) . y
C12 C13 1.386(3) . y
C13 C14 1.388(2) . y
