#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/37/2223737.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_2223737
loop_
_publ_author_name
'Guo, Meng'
_publ_section_title
;
 Tetraaqua(4,5-diazafluoren-9-one-κ²N,N')nickel(II)
 dinitrate
;
_journal_coeditor_code           FI2084
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1361
_journal_paper_doi               10.1107/S1600536809041221
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C11 H6 N2 O) (H2 O)4] (N O3)2'
_chemical_formula_moiety         'C11 H14 N2 Ni O5 2+, 2(N O3 -)'
_chemical_formula_sum            'C11 H14 N4 Ni O11'
_chemical_formula_weight         436.97
_chemical_name_systematic
;
Tetraaqua(4,5-diazafluoren-9-one-κ²N,N')nickel(II) dinitrate
;
_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                 105.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.904(3)
_cell_length_b                   10.207(2)
_cell_length_c                   13.084(3)
_cell_measurement_reflns_used    1023
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.58
_cell_volume                     1657.8(7)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  '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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4262
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.7895
_exptl_absorpt_correction_T_min  0.7386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.603
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0363
_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)+(0.0607P)²+2.0108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                1303
_reflns_number_total             1465
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fi2084.cif
_cod_data_source_block           I
_cod_original_cell_volume        1657.8(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2223737
_cod_database_fobs_code          2223737
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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.0000 0.25222(4) 0.2500 0.0324(2) Uani d S 1 . .
O O4 0.0000 0.8551(3) 0.2500 0.0626(9) Uani d S 1 . .
N N2 0.06304(18) 0.4111(2) 0.35714(17) 0.0364(5) Uani d . 1 . .
C C1 0.1215(2) 0.4279(3) 0.4587(2) 0.0457(7) Uani d . 1 . .
H H1A 0.1466 0.3544 0.5000 0.055 Uiso calc R 1 . .
C C2 0.1455(3) 0.5512(3) 0.5037(2) 0.0532(8) Uani d . 1 . .
H H2A 0.1856 0.5581 0.5742 0.064 Uiso calc R 1 . .
C C3 0.1109(2) 0.6640(3) 0.4459(2) 0.0509(7) Uani d . 1 . .
H H3A 0.1265 0.7467 0.4759 0.061 Uiso calc R 1 . .
C C4 0.0525(2) 0.6478(3) 0.3418(2) 0.0398(6) Uani d . 1 . .
C C5 0.0318(2) 0.5207(2) 0.3050(2) 0.0338(6) Uani d . 1 . .
C C6 0.0000 0.7384(4) 0.2500 0.0452(10) Uani d S 1 . .
O O1W 0.13445(18) 0.24757(16) 0.19659(18) 0.0457(5) Uani d . 1 . .
H H1W1 0.1848 0.2789 0.1735 0.055 Uiso d R 1 . .
H H2W1 0.1543 0.1723 0.2223 0.055 Uiso d R 1 . .
O O2W 0.07053(17) 0.11039(19) 0.35806(16) 0.0494(5) Uani d . 1 . .
H H1W2 0.1031 0.0988 0.4233 0.059 Uiso d R 1 . .
H H2W2 0.0398 0.0387 0.3341 0.059 Uiso d R 1 . .
N N1 0.1702(2) 0.9279(3) 0.1387(2) 0.0557(7) Uani d . 1 . .
O O1 0.2159(2) 0.9812(3) 0.2222(2) 0.0748(8) Uani d . 1 . .
O O2 0.1842(2) 0.8094(3) 0.1304(3) 0.0966(11) Uani d . 1 . .
O O3 0.1130(3) 0.9928(4) 0.0676(2) 0.1121(13) Uani d . 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
O1W Ni1 O1W 2 . 177.33(10) ?
O1W Ni1 O2W 2 2 87.77(8) ?
O1W Ni1 O2W . 2 90.35(9) ?
O1W Ni1 O2W 2 . 90.35(9) ?
O1W Ni1 O2W . . 87.77(8) ?
O2W Ni1 O2W 2 . 90.39(12) ?
O1W Ni1 O2W 2 1 90.35(9) ?
O1W Ni1 O2W . 1 87.77(8) ?
O2W Ni1 O2W 2 1 90.39(12) ?
O2W Ni1 O2W . 1 0.00(12) ?
O1W Ni1 N2 2 . 89.99(8) ?
O1W Ni1 N2 . . 92.01(8) ?
O2W Ni1 N2 2 . 175.31(8) ?
O2W Ni1 N2 . . 93.74(9) ?
O2W Ni1 N2 1 . 93.74(9) ?
O1W Ni1 N2 2 2 92.01(8) ?
O1W Ni1 N2 . 2 89.99(8) ?
O2W Ni1 N2 2 2 93.74(9) ?
O2W Ni1 N2 . 2 175.31(8) ?
O2W Ni1 N2 1 2 175.31(8) ?
N2 Ni1 N2 . 2 82.22(12) ?
C5 N2 C1 . . 114.4(2) ?
C5 N2 Ni1 . . 107.21(16) ?
C1 N2 Ni1 . . 138.41(19) ?
N2 C1 C2 . . 122.2(3) ?
N2 C1 H1A . . 118.9 ?
C2 C1 H1A . . 118.9 ?
C3 C2 C1 . . 121.5(3) ?
C3 C2 H2A . . 119.3 ?
C1 C2 H2A . . 119.3 ?
C4 C3 C2 . . 116.7(3) ?
C4 C3 H3A . . 121.7 ?
C2 C3 H3A . . 121.7 ?
C3 C4 C5 . . 117.3(3) ?
C3 C4 C6 . . 135.6(3) ?
C5 C4 C6 . . 107.1(2) ?
N2 C5 C4 . . 127.9(2) ?
N2 C5 C5 . 2 121.67(14) ?
C4 C5 C5 . 2 110.40(16) ?
O4 C6 C4 . 2 127.46(15) ?
O4 C6 C4 . . 127.46(15) ?
C4 C6 C4 2 . 105.1(3) ?
Ni1 O1W H1W1 . . 156.5 ?
Ni1 O1W H2W1 . . 94.5 ?
H1W1 O1W H2W1 . . 107.7 ?
O2W O2W Ni1 1 . 0(10) ?
O2W O2W H1W2 1 . 0.0 ?
Ni1 O2W H1W2 . . 142.5 ?
O2W O2W H2W2 1 . 0.0 ?
Ni1 O2W H2W2 . . 106.1 ?
H1W2 O2W H2W2 . . 107.7 ?
O3 N1 O1 . . 119.1(3) ?
O3 N1 O2 . . 122.8(3) ?
O1 N1 O2 . . 118.1(3) ?
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 O1W 2 2.040(2) ?
Ni1 O1W . 2.040(2) ?
Ni1 O2W 2 2.054(2) ?
Ni1 O2W . 2.054(2) ?
Ni1 O2W 1 2.054(2) ?
Ni1 N2 . 2.153(2) ?
Ni1 N2 2 2.153(2) ?
O4 C6 . 1.191(4) ?
N2 C5 . 1.315(3) ?
N2 C1 . 1.347(4) ?
C1 C2 . 1.388(4) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.382(5) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.374(4) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.383(3) ?
C4 C6 . 1.521(4) ?
C5 C5 2 1.450(5) ?
C6 C4 2 1.521(4) ?
O1W H1W1 . 0.8502 ?
O1W H2W1 . 0.8501 ?
O2W O2W 1 0.000(4) ?
O2W H1W2 . 0.8501 ?
O2W H2W2 . 0.8500 ?
N1 O3 . 1.214(4) ?
N1 O1 . 1.219(4) ?
N1 O2 . 1.231(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H2W1 O2W 1 0.85 2.40 2.838(3) 113
O1W H1W1 O1 4_545 0.85 2.61 3.070(3) 115
O1W H2W1 O1 1_545 0.85 2.11 2.901(3) 156
O2W H1W2 O3 6_566 0.85 2.08 2.848(4) 150
O2W H2W2 O4 1_545 0.85 2.16 2.986(3) 163
