#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/47/1514783.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_1514783
loop_
_publ_author_name
'Williams, Valerie A.'
'Hulley, Elliott B.'
'Wolczanski, Peter T.'
'Lancaster, Kyle M.'
'Lobkovsky, Emil B.'
_publ_section_title
;
 Exploring the limits of redox non-innocence: pseudo square planar
 [{κ4-Me2C(CH2NCHpy)2}Ni]n (n = 2+, 1+, 0, −1, −2)
 favor Ni(ii)
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3636
_journal_paper_doi               10.1039/c3sc50743b
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C17 H20 N4 Ni'
_chemical_formula_sum            'C17 H20 N4 Ni'
_chemical_formula_weight         339.08
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.463(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9461(4)
_cell_length_b                   7.3243(2)
_cell_length_c                   15.6793(4)
_cell_measurement_reflns_used    4316
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.63
_cell_volume                     1586.18(8)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14568
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.9413
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            parallelepiped
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       black
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0555P)²+0.0436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                3240
_reflns_number_total             3949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc50743b.txt
_cod_data_source_block           eh10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1586.18(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1514783
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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 0.275695(11) 0.68861(2) 0.140394(12) 0.02050(5) Uani 1 1 d .
N1 N 0.24613(8) 0.44506(16) 0.09496(8) 0.0226(3) Uani 1 1 d .
N2 N 0.14733(8) 0.68996(16) 0.13093(8) 0.0227(3) Uani 1 1 d .
N3 N 0.32050(8) 0.87108(17) 0.23076(8) 0.0233(3) Uani 1 1 d .
N4 N 0.38715(8) 0.75144(17) 0.11585(8) 0.0217(3) Uani 1 1 d .
C1 C 0.30143(11) 0.3186(2) 0.07464(11) 0.0257(3) Uani 1 1 d .
C2 C 0.26680(12) 0.1554(2) 0.03362(11) 0.0296(4) Uani 1 1 d .
C3 C 0.16941(12) 0.1110(2) 0.01130(11) 0.0314(4) Uani 1 1 d .
C4 C 0.11186(11) 0.2328(2) 0.03272(11) 0.0292(4) Uani 1 1 d .
C5 C 0.15087(10) 0.3993(2) 0.07529(10) 0.0240(3) Uani 1 1 d .
C6 C 0.10039(10) 0.5350(2) 0.10279(10) 0.0237(3) Uani 1 1 d .
C7 C 0.10665(10) 0.8243(2) 0.17480(11) 0.0265(3) Uani 1 1 d .
C8 C 0.17513(11) 0.8641(2) 0.27502(11) 0.0307(4) Uani 1 1 d .
C9 C 0.26482(11) 0.9663(2) 0.27660(11) 0.0303(4) Uani 1 1 d .
C10 C 0.40229(10) 0.9505(2) 0.23617(10) 0.0255(3) Uani 1 1 d .
C11 C 0.44447(10) 0.8808(2) 0.17639(10) 0.0232(3) Uani 1 1 d .
C12 C 0.53203(11) 0.9394(2) 0.17242(11) 0.0286(3) Uani 1 1 d .
C13 C 0.56133(11) 0.8706(2) 0.10641(11) 0.0313(4) Uani 1 1 d .
C14 C 0.50304(11) 0.7409(2) 0.04422(11) 0.0294(3) Uani 1 1 d .
C15 C 0.41944(11) 0.68536(19) 0.05174(11) 0.0243(3) Uani 1 1 d .
C16 C 0.20211(13) 0.6874(3) 0.33055(12) 0.0415(5) Uani 1 1 d .
H16A H 0.1430 0.6230 0.3262 0.062 Uiso 1 1 calc R
H16B H 0.2408 0.7158 0.3953 0.062 Uiso 1 1 calc R
H16C H 0.2399 0.6097 0.3058 0.062 Uiso 1 1 calc R
C17 C 0.12058(13) 0.9915(3) 0.31631(13) 0.0509(5) Uani 1 1 d .
H17A H 0.1009 1.1022 0.2786 0.076 Uiso 1 1 calc R
H17B H 0.1630 1.0247 0.3794 0.076 Uiso 1 1 calc R
H17C H 0.0630 0.9289 0.3173 0.076 Uiso 1 1 calc R
H1 H 0.3704(11) 0.351(2) 0.0952(11) 0.025(4) Uiso 1 1 d .
H15 H 0.3790(10) 0.601(2) 0.0123(10) 0.014(4) Uiso 1 1 d .
H7B H 0.0448(11) 0.778(2) 0.1732(11) 0.020(4) Uiso 1 1 d .
H10 H 0.4274(11) 1.055(2) 0.2730(11) 0.028(4) Uiso 1 1 d .
H6 H 0.0376(11) 0.512(2) 0.1042(11) 0.024(4) Uiso 1 1 d .
H7A H 0.0924(10) 0.942(2) 0.1376(10) 0.018(4) Uiso 1 1 d .
H9B H 0.2431(10) 1.089(2) 0.2475(10) 0.023(4) Uiso 1 1 d .
H13 H 0.6184(12) 0.900(2) 0.1042(12) 0.035(5) Uiso 1 1 d .
H2 H 0.3087(11) 0.068(2) 0.0204(11) 0.028(4) Uiso 1 1 d .
H12 H 0.5667(11) 1.023(2) 0.2095(11) 0.026(4) Uiso 1 1 d .
H4 H 0.0425(13) 0.209(2) 0.0209(12) 0.031(5) Uiso 1 1 d .
H14 H 0.5189(14) 0.698(2) -0.0025(15) 0.045(6) Uiso 1 1 d .
H3 H 0.1425(13) -0.004(3) -0.0163(13) 0.045(6) Uiso 1 1 d .
H9A H 0.3092(12) 0.987(2) 0.3402(13) 0.036(5) 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'
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
N2 Ni1 N3 96.65(5)
N2 Ni1 N4 159.17(5)
N3 Ni1 N4 83.86(5)
N2 Ni1 N1 83.74(5)
N3 Ni1 N1 155.89(5)
N4 Ni1 N1 104.25(5)
C1 N1 C5 116.82(12)
C1 N1 Ni1 130.54(10)
C5 N1 Ni1 112.51(10)
C6 N2 C7 118.29(13)
C6 N2 Ni1 114.91(10)
C7 N2 Ni1 124.51(9)
C10 N3 C9 116.19(13)
C10 N3 Ni1 114.53(10)
C9 N3 Ni1 127.10(10)
C15 N4 C11 116.73(12)
C15 N4 Ni1 130.44(10)
C11 N4 Ni1 112.79(10)
N1 C1 C2 123.62(14)
C1 C2 C3 119.57(15)
C4 C3 C2 118.60(15)
C3 C4 C5 119.80(15)
N1 C5 C4 121.54(14)
N1 C5 C6 112.81(12)
C4 C5 C6 125.65(14)
N2 C6 C5 115.49(13)
N2 C7 C8 111.97(12)
C16 C8 C9 111.56(13)
C16 C8 C17 110.00(15)
C9 C8 C17 107.45(14)
C16 C8 C7 110.43(14)
C9 C8 C7 110.26(13)
C17 C8 C7 106.98(13)
N3 C9 C8 114.71(13)
N3 C10 C11 115.70(13)
N4 C11 C12 121.58(14)
N4 C11 C10 112.79(13)
C12 C11 C10 125.54(14)
C13 C12 C11 119.76(14)
C12 C13 C14 118.93(15)
C15 C14 C13 119.31(15)
N4 C15 C14 123.68(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 N2 1.8670(12)
Ni1 N3 1.8754(12)
Ni1 N4 1.9038(12)
Ni1 N1 1.9091(12)
N1 C1 1.3577(19)
N1 C5 1.3780(18)
N2 C6 1.3186(18)
N2 C7 1.4599(19)
N3 C10 1.3269(19)
N3 C9 1.467(2)
N4 C15 1.360(2)
N4 C11 1.3827(18)
C1 C2 1.362(2)
C2 C3 1.399(2)
C3 C4 1.367(2)
C4 C5 1.405(2)
C5 C6 1.411(2)
C7 C8 1.540(2)
C8 C16 1.526(3)
C8 C9 1.527(2)
C8 C17 1.535(2)
C10 C11 1.410(2)
C11 C12 1.401(2)
C12 C13 1.365(2)
C13 C14 1.401(2)
C14 C15 1.361(2)
