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#$Date: 2016-03-05 11:58:39 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177826 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/79/7037979.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_7037979
loop_
_publ_author_name
'Nyamato, George S.'
'Ojwach, Stephen O.'
'Akerman, Matthew P.'
_publ_section_title
;
 Ethylene oligomerization studies by nickel(ii) complexes chelated by
 (amino)pyridine ligands: experimental and density functional theory
 studies.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3407
_journal_page_last               3416
_journal_paper_doi               10.1039/c5dt04667j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C16 H24 N4 Ni O2, 2(Br), 2(H2 O)'
_chemical_formula_sum            'C16 H28 Br2 N4 Ni O4'
_chemical_formula_weight         558.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-10 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                109.596(2)
_cell_angle_beta                 98.327(2)
_cell_angle_gamma                101.729(2)
_cell_formula_units_Z            1
_cell_length_a                   8.1950(4)
_cell_length_b                   8.3725(4)
_cell_length_c                   8.9081(4)
_cell_measurement_reflns_used    2119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      2.5
_cell_volume                     548.55(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2012)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7914
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.087
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'Incoatec microsource'
_exptl_absorpt_coefficient_mu    4.554
_exptl_absorpt_correction_T_max  0.6947
_exptl_absorpt_correction_T_min  0.2570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker 2012'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       needle
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0338P)²+0.3159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1955
_reflns_number_total             2119
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt04667j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7037978--7037979.cif.'
_cod_database_code               7037979
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.478
_shelx_estimated_absorpt_t_max   0.839
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br2 Br 0.28354(3) 0.31066(3) 0.07519(3) 0.02125(10) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.0000 0.5000 0.01230(11) Uani 1 2 d S . P
O1W O 0.5161(2) 0.7253(3) 0.2221(2) 0.0250(4) Uani 1 1 d . . .
C1 C 0.1988(3) -0.1360(3) 0.7303(3) 0.0183(5) Uani 1 1 d . . .
H1 H 0.1898 -0.0373 0.8176 0.022 Uiso 1 1 calc R U .
O1 O -0.2409(2) -0.1507(2) 0.5001(2) 0.0182(4) Uani 1 1 d . . .
N2 N 0.0217(2) -0.1619(3) 0.2727(2) 0.0148(4) Uani 1 1 d . . .
N1 N 0.1233(2) -0.1632(3) 0.5755(2) 0.0151(4) Uani 1 1 d . . .
C8 C -0.3094(3) -0.0457(3) 0.6267(3) 0.0209(5) Uani 1 1 d . . .
H8A H -0.3975 -0.1224 0.6559 0.025 Uiso 1 1 calc R U .
H8B H -0.3628 0.0340 0.5885 0.025 Uiso 1 1 calc R U .
C7 C 0.1621(3) -0.0598(3) 0.2268(3) 0.0205(5) Uani 1 1 d . . .
H7B H 0.1187 0.0207 0.1818 0.025 Uiso 1 1 calc R U .
H7A H 0.2026 -0.1413 0.1407 0.025 Uiso 1 1 calc R U .
C6 C 0.0490(3) -0.3279(3) 0.2816(3) 0.0191(5) Uani 1 1 d . . .
H6B H 0.1201 -0.3724 0.2048 0.023 Uiso 1 1 calc R U .
H6A H -0.0629 -0.4172 0.2472 0.023 Uiso 1 1 calc R U .
C5 C 0.1365(3) -0.3029(3) 0.4531(3) 0.0154(5) Uani 1 1 d . . .
C2 C 0.2889(3) -0.2466(3) 0.7665(3) 0.0196(5) Uani 1 1 d . . .
H2 H 0.3419 -0.2233 0.8765 0.024 Uiso 1 1 calc R U .
C3 C 0.3006(3) -0.3915(3) 0.6399(3) 0.0210(5) Uani 1 1 d . . .
H3 H 0.3617 -0.4692 0.6620 0.025 Uiso 1 1 calc R U .
C4 C 0.2221(3) -0.4220(3) 0.4803(3) 0.0201(5) Uani 1 1 d . . .
H4 H 0.2265 -0.5219 0.3915 0.024 Uiso 1 1 calc R U .
H2W H 0.556(6) 0.716(6) 0.144(5) 0.070(14) Uiso 1 1 d . . .
H1W H 0.453(5) 0.621(5) 0.190(4) 0.042(10) Uiso 1 1 d . . .
H101 H -0.062(3) -0.193(3) 0.197(3) 0.013(6) Uiso 1 1 d . . .
H102 H -0.303(4) -0.177(4) 0.428(4) 0.022(8) Uiso 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'
Br Br -0.2901 2.4595 '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
N1 Ni1 N1 180.0 2_556 .
N1 Ni1 N2 98.71(7) 2_556 .
N1 Ni1 N2 81.29(7) . .
N1 Ni1 N2 81.29(7) 2_556 2_556
N1 Ni1 N2 98.71(7) . 2_556
N2 Ni1 N2 180.0 . 2_556
N1 Ni1 O1 91.06(7) 2_556 2_556
N1 Ni1 O1 88.94(7) . 2_556
N2 Ni1 O1 82.50(7) . 2_556
N2 Ni1 O1 97.50(7) 2_556 2_556
N1 Ni1 O1 88.94(7) 2_556 .
N1 Ni1 O1 91.06(7) . .
N2 Ni1 O1 97.50(7) . .
N2 Ni1 O1 82.50(7) 2_556 .
O1 Ni1 O1 180.0 2_556 .
H2W O1W H1W 99(4) . .
N1 C1 C2 122.3(2) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C8 O1 Ni1 109.28(14) . .
C8 O1 H102 105(2) . .
Ni1 O1 H102 115(3) . .
C6 N2 C7 113.99(18) . .
C6 N2 Ni1 109.61(14) . .
C7 N2 Ni1 107.02(15) . .
C6 N2 H101 104.8(18) . .
C7 N2 H101 105.5(18) . .
Ni1 N2 H101 116.0(18) . .
C5 N1 C1 118.44(19) . .
C5 N1 Ni1 114.51(14) . .
C1 N1 Ni1 126.89(16) . .
O1 C8 C7 107.26(19) . 2_556
O1 C8 H8A 110.3 . .
C7 C8 H8A 110.3 2_556 .
O1 C8 H8B 110.3 . .
C7 C8 H8B 110.3 2_556 .
H8A C8 H8B 108.5 . .
N2 C7 C8 110.85(19) . 2_556
N2 C7 H7B 109.5 . .
C8 C7 H7B 109.5 2_556 .
N2 C7 H7A 109.5 . .
C8 C7 H7A 109.5 2_556 .
H7B C7 H7A 108.1 . .
N2 C6 C5 111.81(19) . .
N2 C6 H6B 109.3 . .
C5 C6 H6B 109.3 . .
N2 C6 H6A 109.3 . .
C5 C6 H6A 109.3 . .
H6B C6 H6A 107.9 . .
N1 C5 C4 122.5(2) . .
N1 C5 C6 116.3(2) . .
C4 C5 C6 121.2(2) . .
C3 C2 C1 119.0(2) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C2 C3 C4 119.2(2) . .
C2 C3 H3 120.4 . .
C4 C3 H3 120.4 . .
C3 C4 C5 118.5(2) . .
C3 C4 H4 120.8 . .
C5 C4 H4 120.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.0792(18) 2_556
Ni1 N1 2.0792(18) .
Ni1 N2 2.0806(19) .
Ni1 N2 2.0806(19) 2_556
Ni1 O1 2.1161(17) 2_556
Ni1 O1 2.1161(17) .
O1W H2W 0.80(5) .
O1W H1W 0.85(4) .
C1 N1 1.349(3) .
C1 C2 1.384(3) .
C1 H1 0.9500 .
O1 C8 1.442(3) .
O1 H102 0.70(3) .
N2 C6 1.477(3) .
N2 C7 1.481(3) .
N2 H101 0.82(3) .
N1 C5 1.341(3) .
C8 C7 1.509(3) 2_556
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C7 C8 1.509(3) 2_556
C7 H7B 0.9900 .
C7 H7A 0.9900 .
C6 C5 1.516(3) .
C6 H6B 0.9900 .
C6 H6A 0.9900 .
C5 C4 1.394(3) .
C2 C3 1.383(4) .
C2 H2 0.9500 .
C3 C4 1.388(3) .
C3 H3 0.9500 .
C4 H4 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C2 C1 N1 C5 0.1(3) .
C2 C1 N1 Ni1 -175.03(17) .
Ni1 O1 C8 C7 -39.5(2) 2_556
C6 N2 C7 C8 -81.0(2) 2_556
Ni1 N2 C7 C8 40.4(2) 2_556
C7 N2 C6 C5 92.3(2) .
Ni1 N2 C6 C5 -27.6(2) .
C1 N1 C5 C4 1.3(3) .
Ni1 N1 C5 C4 176.98(17) .
C1 N1 C5 C6 179.8(2) .
Ni1 N1 C5 C6 -4.5(2) .
N2 C6 C5 N1 21.8(3) .
N2 C6 C5 C4 -159.6(2) .
N1 C1 C2 C3 -0.8(4) .
C1 C2 C3 C4 0.1(4) .
C2 C3 C4 C5 1.2(4) .
N1 C5 C4 C3 -1.9(4) .
C6 C5 C4 C3 179.6(2) .
