#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/57/2235716.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2235716
loop_
_publ_author_name
'Wöhlert, Susanne'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Bis(cyanato-κN)tetrakis(2,6-dimethylpyrazine-κN⁴)nickel(II)
;
_journal_coeditor_code           ZL2488
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m970
_journal_paper_doi               10.1107/S1600536812027985
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (N C O)2 (C6 H8 N2)4]'
_chemical_formula_moiety         'C26 H32 N10 Ni O2'
_chemical_formula_sum            'C26 H32 N10 Ni O2'
_chemical_formula_weight         575.33
_chemical_name_systematic
;
Bis(cyanato-κN)tetrakis(2,6-dimethylpyrazine-κN⁴)nickel(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.148(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.932(2)
_cell_length_b                   8.4963(3)
_cell_length_c                   18.1748(13)
_cell_measurement_reflns_used    8293
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.65
_cell_volume                     2808.9(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'omega scan'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8293
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.8879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0386
_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)+(0.0632P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                2516
_reflns_number_total             3341
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2488.cif
_cod_data_source_block           I
_cod_original_cell_volume        2808.9(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2235716
_cod_database_fobs_code          2235716
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ni Ni1 0.7500 0.7500 0.5000 0.01887(11) Uani d S 1 2
N N20 0.64456(8) 0.8103(2) 0.34913(11) 0.0212(3) Uani d . 1 1
N N10 0.79329(8) 0.6983(2) 0.43337(11) 0.0231(4) Uani d . 1 1
C C1 0.68822(10) 0.4093(3) 0.46580(14) 0.0255(4) Uani d . 1 1
N N1 0.71677(9) 0.5219(2) 0.47971(13) 0.0275(4) Uani d . 1 1
N N21 0.50923(9) 0.8818(2) 0.15700(13) 0.0270(4) Uani d . 1 1
C C10 0.82299(10) 0.5593(3) 0.44444(15) 0.0261(4) Uani d . 1 1
H H10 0.8239 0.4804 0.4807 0.031 Uiso calc R 1 1
C C23 0.62225(10) 0.9586(2) 0.31901(15) 0.0237(4) Uani d . 1 1
H H23 0.6526 1.0401 0.3631 0.028 Uiso calc R 1 1
N N11 0.85370(10) 0.6399(3) 0.35157(14) 0.0364(5) Uani d . 1 1
C C22 0.55452(10) 0.9952(3) 0.22309(15) 0.0251(4) Uani d . 1 1
C C20 0.59907(10) 0.6966(3) 0.28228(14) 0.0239(4) Uani d . 1 1
H H20 0.6130 0.5918 0.3002 0.029 Uiso calc R 1 1
O O1 0.65623(11) 0.2844(2) 0.45025(18) 0.0568(6) Uani d . 1 1
C C11 0.85283(11) 0.5294(3) 0.40292(15) 0.0312(5) Uani d . 1 1
C C13 0.79369(10) 0.8085(3) 0.38110(14) 0.0267(4) Uani d . 1 1
H H13 0.7725 0.9060 0.3708 0.032 Uiso calc R 1 1
C C12 0.82493(11) 0.7812(3) 0.34183(16) 0.0330(5) Uani d . 1 1
C C14 0.88376(15) 0.3709(3) 0.4124(2) 0.0454(6) Uani d . 1 1
H H14A 0.8580 0.3295 0.3464 0.068 Uiso calc R 1 1
H H14B 0.8780 0.3006 0.4479 0.068 Uiso calc R 1 1
H H14C 0.9350 0.3812 0.4490 0.068 Uiso calc R 1 1
C C15 0.82941(15) 0.9083(4) 0.2884(2) 0.0526(8) Uani d . 1 1
H H15A 0.8799 0.9357 0.3276 0.079 Uiso calc R 1 1
H H15B 0.8029 0.9994 0.2800 0.079 Uiso calc R 1 1
H H15C 0.8082 0.8707 0.2234 0.079 Uiso calc R 1 1
C C21 0.53149(10) 0.7326(3) 0.18668(14) 0.0272(4) Uani d . 1 1
C C25 0.53126(11) 1.1627(3) 0.19022(17) 0.0341(5) Uani d . 1 1
H H25A 0.5382 1.1915 0.1461 0.051 Uiso calc R 1 1
H H25B 0.5604 1.2302 0.2483 0.051 Uiso calc R 1 1
H H25C 0.4803 1.1738 0.1552 0.051 Uiso calc R 1 1
C C24 0.48127(12) 0.6054(3) 0.11260(18) 0.0405(6) Uani d . 1 1
H H24A 0.4342 0.6160 0.0917 0.061 Uiso calc R 1 1
H H24B 0.5019 0.5045 0.1437 0.061 Uiso calc R 1 1
H H24C 0.4756 0.6143 0.0549 0.061 Uiso calc R 1 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 7_666 . 180.00(13) ?
N1 Ni1 N10 7_666 . 89.86(7) ?
N1 Ni1 N10 . . 90.14(7) n
N1 Ni1 N10 7_666 7_666 90.14(7) ?
N1 Ni1 N10 . 7_666 89.86(7) ?
N10 Ni1 N10 . 7_666 180.000 ?
N1 Ni1 N20 7_666 . 89.74(7) ?
N1 Ni1 N20 . . 90.26(7) n
N10 Ni1 N20 . . 88.72(6) n
N10 Ni1 N20 7_666 . 91.28(6) ?
N1 Ni1 N20 7_666 7_666 90.26(7) ?
N1 Ni1 N20 . 7_666 89.74(7) ?
N10 Ni1 N20 . 7_666 91.28(6) ?
N10 Ni1 N20 7_666 7_666 88.72(6) n
N20 Ni1 N20 . 7_666 180.000 n
C23 N20 C20 . . 116.73(16) ?
C23 N20 Ni1 . . 122.62(13) ?
C20 N20 Ni1 . . 120.64(14) ?
C10 N10 C13 . . 116.95(19) ?
C10 N10 Ni1 . . 122.49(14) ?
C13 N10 Ni1 . . 120.51(15) ?
N1 C1 O1 . . 179.7(2) ?
C1 N1 Ni1 . . 167.16(17) ?
C22 N21 C21 . . 117.19(17) ?
N10 C10 C11 . . 121.7(2) ?
N10 C10 H10 . . 119.2 ?
C11 C10 H10 . . 119.2 ?
N20 C23 C22 . . 122.01(19) ?
N20 C23 H23 . . 119.0 ?
C22 C23 H23 . . 119.0 ?
C11 N11 C12 . . 117.2(2) ?
N21 C22 C23 . . 121.1(2) ?
N21 C22 C25 . . 117.86(17) ?
C23 C22 C25 . . 121.1(2) ?
N20 C20 C21 . . 121.5(2) ?
N20 C20 H20 . . 119.3 ?
C21 C20 H20 . . 119.3 ?
N11 C11 C10 . . 121.2(2) ?
N11 C11 C14 . . 117.3(2) ?
C10 C11 C14 . . 121.5(2) ?
N10 C13 C12 . . 121.8(2) ?
N10 C13 H13 . . 119.1 ?
C12 C13 H13 . . 119.1 ?
N11 C12 C13 . . 121.1(2) ?
N11 C12 C15 . . 117.1(2) ?
C13 C12 C15 . . 121.7(2) ?
C11 C14 H14A . . 109.5 ?
C11 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C11 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C12 C15 H15A . . 109.5 ?
C12 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C12 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N21 C21 C20 . . 121.5(2) ?
N21 C21 C24 . . 117.32(18) ?
C20 C21 C24 . . 121.1(2) ?
C22 C25 H25A . . 109.5 ?
C22 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C22 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C21 C24 H24A . . 109.5 ?
C21 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C21 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 7_666 2.0396(19) ?
Ni1 N1 . 2.0396(19) y
Ni1 N10 . 2.1475(17) y
Ni1 N10 7_666 2.1475(17) ?
Ni1 N20 . 2.1983(15) y
Ni1 N20 7_666 2.1983(15) ?
N20 C23 . 1.335(3) ?
N20 C20 . 1.345(3) ?
N10 C10 . 1.334(3) ?
N10 C13 . 1.339(3) ?
C1 N1 . 1.113(3) ?
C1 O1 . 1.238(3) ?
N21 C22 . 1.339(3) ?
N21 C21 . 1.341(3) ?
C10 C11 . 1.398(3) ?
C10 H10 . 0.9300 ?
C23 C22 . 1.400(3) ?
C23 H23 . 0.9300 ?
N11 C11 . 1.334(3) ?
N11 C12 . 1.347(3) ?
C22 C25 . 1.498(3) ?
C20 C21 . 1.395(3) ?
C20 H20 . 0.9300 ?
C11 C14 . 1.502(3) ?
C13 C12 . 1.389(3) ?
C13 H13 . 0.9300 ?
C12 C15 . 1.507(3) ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
C21 C24 . 1.497(3) ?
C25 H25A . 0.9600 ?
C25 H25B . 0.9600 ?
C25 H25C . 0.9600 ?
C24 H24A . 0.9600 ?
C24 H24B . 0.9600 ?
C24 H24C . 0.9600 ?
