#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/99/2229922.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_2229922
loop_
_publ_author_name
'Wöhlert, Susanne'
'Wriedt, Mario'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Poly[aquabis(μ-formato-κ²O:O')(μ-pyrazine-κ²N:N')nickel(II)]
;
_journal_coeditor_code           BT5501
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m532
_journal_paper_doi               10.1107/S1600536811011913
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C H O2)2 (C4 H4 N2) (H2 O)]'
_chemical_formula_moiety         'C6 H8 N2 Ni O5'
_chemical_formula_sum            'C6 H8 N2 Ni O5'
_chemical_formula_weight         246.85
_chemical_name_systematic
;
Poly[aquabis(μ-formato-κ²O:O')(μ-
pyrazine-κ²N:N')nickel(II)]
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.971(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8169(4)
_cell_length_b                   7.0077(3)
_cell_length_c                   15.6586(7)
_cell_measurement_reflns_used    15596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.64
_cell_volume                     847.26(7)
_computing_cell_refinement       'X-AREA (Stoe, 2008)'
_computing_data_collection       'X-AREA (Stoe, 2008)'
_computing_data_reduction        'X-AREA (Stoe, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2011)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15596
_diffrn_reflns_theta_full        29.25
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.288
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe, 2008)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.297
_refine_ls_extinction_coef       0.0158(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+0.4622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                2091
_reflns_number_total             2291
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            bt5501.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229922
_cod_database_fobs_code          2229922
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_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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.30005(2) 0.25657(3) 0.649349(11) 0.01731(8) Uani d . 1 . .
N N1 0.41659(17) 0.10169(18) 0.55756(8) 0.0205(2) Uani d . 1 . .
C C1 0.3337(2) 0.0453(2) 0.48084(10) 0.0250(3) Uani d . 1 . .
H H1 0.2169 0.0747 0.4654 0.030 Uiso calc R 1 . .
C C2 0.5831(2) 0.0558(2) 0.57642(10) 0.0257(3) Uani d . 1 . .
H H2 0.6452 0.0925 0.6294 0.031 Uiso calc R 1 . .
N N11 0.12229(17) 0.39364(18) 0.55394(8) 0.0209(2) Uani d . 1 . .
C C11 -0.0463(2) 0.3831(2) 0.55924(11) 0.0241(3) Uani d . 1 . .
H H11 -0.0827 0.3027 0.6001 0.029 Uiso calc R 1 . .
C C12 0.1684(2) 0.5112(2) 0.49450(10) 0.0234(3) Uani d . 1 . .
H H12 0.2847 0.5224 0.4891 0.028 Uiso calc R 1 . .
O O21 0.11734(15) 0.04433(16) 0.65066(8) 0.0275(3) Uani d . 1 . .
O O22 0.0548(2) -0.25397(17) 0.67969(12) 0.0434(4) Uani d . 1 . .
C C21 0.1545(2) -0.1280(2) 0.66185(12) 0.0279(3) Uani d . 1 . .
H H21 0.2693 -0.1604 0.6602 0.042 Uiso d R 1 . .
O O31 0.46637(15) 0.11818(18) 0.74213(8) 0.0282(3) Uani d . 1 . .
O O32 0.51992(15) -0.03704(17) 0.86756(7) 0.0260(2) Uani d . 1 . .
C C31 0.4364(2) 0.0746(2) 0.81445(11) 0.0258(3) Uani d . 1 . .
H H31 0.3479 0.1347 0.8375 0.039 Uiso d R 1 . .
O O41 0.18980(15) 0.40396(16) 0.73925(7) 0.0241(2) Uani d . 1 . .
H H1O 0.1126 0.3547 0.7617 0.036 Uiso d R 1 . .
H H2O 0.1500 0.5093 0.7246 0.036 Uiso d R 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
O31 Ni1 O41 . . 92.30(5) ?
O31 Ni1 O32 . 2_656 93.04(5) ?
O41 Ni1 O32 . 2_656 95.94(5) ?
O31 Ni1 O21 . . 90.89(5) ?
O41 Ni1 O21 . . 89.46(5) ?
O32 Ni1 O21 2_656 . 173.18(5) ?
O31 Ni1 N11 . . 178.28(5) ?
O41 Ni1 N11 . . 87.46(5) ?
O32 Ni1 N11 2_656 . 88.68(5) ?
O21 Ni1 N11 . . 87.40(5) ?
O31 Ni1 N1 . . 86.89(5) ?
O41 Ni1 N1 . . 179.19(5) ?
O32 Ni1 N1 2_656 . 84.14(5) ?
O21 Ni1 N1 . . 90.52(5) ?
N11 Ni1 N1 . . 93.35(5) ?
C2 N1 C1 . . 116.76(13) ?
C2 N1 Ni1 . . 118.93(11) ?
C1 N1 Ni1 . . 124.31(10) ?
N1 C1 C2 . 3_656 121.65(14) ?
N1 C1 H1 . . 119.2 ?
C2 C1 H1 3_656 . 119.2 ?
N1 C2 C1 . 3_656 121.59(15) ?
N1 C2 H2 . . 119.2 ?
C1 C2 H2 3_656 . 119.2 ?
C12 N11 C11 . . 117.00(13) ?
C12 N11 Ni1 . . 123.80(11) ?
C11 N11 Ni1 . . 118.62(10) ?
N11 C11 C12 . 3_566 121.75(14) ?
N11 C11 H11 . . 119.1 ?
C12 C11 H11 3_566 . 119.1 ?
N11 C12 C11 . 3_566 121.25(14) ?
N11 C12 H12 . . 119.4 ?
C11 C12 H12 3_566 . 119.4 ?
C21 O21 Ni1 . . 123.54(11) ?
O22 C21 O21 . . 125.53(16) ?
O22 C21 H21 . . 118.4 ?
O21 C21 H21 . . 115.9 ?
C31 O31 Ni1 . . 125.64(11) ?
C31 O32 Ni1 . 2_646 130.50(10) ?
O31 C31 O32 . . 127.86(15) ?
O31 C31 H31 . . 120.4 ?
O32 C31 H31 . . 111.6 ?
Ni1 O41 H1O . . 120.0 ?
Ni1 O41 H2O . . 116.4 ?
H1O O41 H2O . . 103.1 ?
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 O31 . 2.0378(11) ?
Ni1 O41 . 2.0420(11) ?
Ni1 O32 2_656 2.0636(11) ?
Ni1 O21 . 2.0643(12) ?
Ni1 N11 . 2.1066(13) ?
Ni1 N1 . 2.1171(12) ?
N1 C2 . 1.328(2) ?
N1 C1 . 1.333(2) ?
C1 C2 3_656 1.382(2) ?
C1 H1 . 0.9300 ?
C2 C1 3_656 1.382(2) ?
C2 H2 . 0.9300 ?
N11 C12 . 1.334(2) ?
N11 C11 . 1.335(2) ?
C11 C12 3_566 1.385(2) ?
C11 H11 . 0.9300 ?
C12 C11 3_566 1.385(2) ?
C12 H12 . 0.9300 ?
O21 C21 . 1.2479(19) ?
O22 C21 . 1.238(2) ?
C21 H21 . 0.9300 ?
O31 C31 . 1.230(2) ?
O32 C31 . 1.2492(19) ?
O32 Ni1 2_646 2.0636(11) ?
C31 H31 . 0.9299 ?
O41 H1O . 0.8200 ?
O41 H2O . 0.8200 ?
