#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/22/8102237.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_8102237
loop_
_publ_author_name
'Leonore Wiehl'
'Jürgen Schreuer'
'Eiken Haussühl'
_publ_section_title
;
 Crystal structure of triaqua-1,10-phenanthroline-nickel(II) maleate
 dihydrate, Ni(H2O)3(C12H8N2)(C4H2O4) · 2H2O
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              82
_journal_volume                  223
_journal_year                    2008
_chemical_formula_structural     'Ni(H2O)3(C12H8N2)(C4H2O4) &#x00B7; 2 H~2~O'
_chemical_formula_sum            'C16 H20 N2 Ni O9'
_chemical_formula_weight         443.05
_chemical_name_systematic
; 
triaqua-1,10-phenanthroline-nickel(II) maleate dihydrate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.734(8)
_cell_angle_beta                 100.846(9)
_cell_angle_gamma                113.309(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9383(10)
_cell_length_b                   9.3363(9)
_cell_length_c                   13.2143(14)
_cell_measurement_reflns_used    13015
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      4.07
_cell_volume                     957.7(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_molecular_graphics
;   Ortep-3 for Windows (Farrugia) 
    Accelrys MS Modeling 4.0  
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9682
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur3 & Sapphire3 CCD'
_diffrn_measurement_method       phi/omega
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17523
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         4.07
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 
CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics, implemented in 
SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+0.3175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                4014
_reflns_number_total             4673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2182.cff
_cod_data_source_block           nimalephen
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3175P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3175P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        957.71(17)
_cod_database_code               8102237
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.47097(2) 0.29630(2) 0.273819(13) 0.02563(6) Uani 1 2 i d . . .
O1W O 0.62645(17) 0.18743(16) 0.30781(9) 0.0345(2) Uani 1 2 i d . . .
O2W O 0.43875(18) 0.30532(14) 0.42530(9) 0.0345(2) Uani 1 2 i d . . .
O3W O 0.68837(15) 0.51646(14) 0.32132(10) 0.0346(2) Uani 1 2 i d . . .
O4W O 0.5871(2) -0.02176(18) 0.42866(14) 0.0568(4) Uani 1 2 i d . . .
O5W O 0.9337(2) 0.1092(2) 0.52074(15) 0.0669(4) Uani 1 2 i d . . .
H11W H 0.723(3) 0.244(3) 0.3265(17) 0.042(6) Uiso 1 2 i d . . .
H21W H 0.600(3) 0.116(3) 0.346(2) 0.072(8) Uiso 1 2 i d . . .
H12W H 0.371(3) 0.345(3) 0.4389(17) 0.050(6) Uiso 1 2 i d . . .
H22W H 0.531(4) 0.358(3) 0.468(2) 0.080(9) Uiso 1 2 i d . . .
H13W H 0.641(3) 0.578(3) 0.3158(19) 0.058(7) Uiso 1 2 i d . . .
H23W H 0.737(3) 0.540(3) 0.388(2) 0.071(8) Uiso 1 2 i d . . .
H14W H 0.559(3) -0.103(3) 0.397(2) 0.063(8) Uiso 1 2 i d . . .
H24W H 0.5000 0.0000 0.5000 0.23(3) Uiso 1 1 f d S . .
H15W H 0.962(4) 0.165(3) 0.484(2) 0.071(8) Uiso 1 1 b d . . .
H25W H 1.0000 0.0000 0.5000 0.27(4) Uiso 1 2 i d S . .
H35W H 0.762(8) 0.028(6) 0.473(4) 0.21(2) Uiso 1 2 i d . . .
N1 N 0.47436(17) 0.24993(16) 0.11540(9) 0.0321(3) Uani 1 2 i d . . .
N2 N 0.25677(16) 0.07505(14) 0.21139(10) 0.0289(2) Uani 1 2 i d . . .
C1 C 0.3435(2) 0.10857(19) 0.05333(11) 0.0322(3) Uani 1 2 i d . . .
C2 C 0.5849(3) 0.3373(3) 0.07046(15) 0.0492(4) Uani 1 2 i d . . .
C3 C 0.5691(3) 0.2899(3) -0.03897(16) 0.0636(6) Uani 1 2 i d . . .
C4 C 0.4386(3) 0.1496(3) -0.10176(15) 0.0593(6) Uani 1 2 i d . . .
C5 C 0.1745(3) -0.0960(3) -0.11651(15) 0.0557(5) Uani 1 2 i d . . .
C6 C 0.0628(3) -0.1807(3) -0.06928(16) 0.0558(5) Uani 1 2 i d . . .
C7 C -0.0276(3) -0.2110(2) 0.09847(19) 0.0519(5) Uani 1 2 i d . . .
C8 C 0.0035(3) -0.1514(2) 0.20539(18) 0.0497(4) Uani 1 2 i d . . .
C9 C 0.1482(2) -0.0071(2) 0.26003(14) 0.0393(4) Uani 1 2 i d . . .
C10 C 0.2253(2) 0.01537(18) 0.10465(12) 0.0317(3) Uani 1 2 i d . . .
C11 C 0.3192(3) 0.0526(2) -0.05691(12) 0.0438(4) Uani 1 2 i d . . .
C12 C 0.0845(2) -0.1289(2) 0.04380(14) 0.0426(4) Uani 1 2 i d . . .
H2 H 0.677(3) 0.438(3) 0.1176(18) 0.055(6) Uiso 1 2 i d . . .
H3 H 0.654(3) 0.358(3) -0.065(2) 0.072(7) Uiso 1 2 i d . . .
H4 H 0.428(3) 0.115(3) -0.1730(19) 0.062(6) Uiso 1 2 i d . . .
H5 H 0.165(3) -0.130(3) -0.188(2) 0.065(7) Uiso 1 2 i d . . .
H6 H -0.033(3) -0.277(3) -0.1065(19) 0.060(6) Uiso 1 2 i d . . .
H7 H -0.120(3) -0.298(3) 0.0646(18) 0.051(6) Uiso 1 2 i d . . .
H8 H -0.067(3) -0.200(3) 0.2427(19) 0.058(6) Uiso 1 2 i d . . .
H9 H 0.178(2) 0.038(2) 0.3343(16) 0.039(5) Uiso 1 2 i d . . .
O1M O 0.31688(14) 0.40984(13) 0.24695(9) 0.0334(2) Uani 1 2 i d . . .
O2M O 0.49931(16) 0.67141(14) 0.30285(12) 0.0474(3) Uani 1 2 i d . . .
O3M O 0.24206(14) 0.46287(15) 0.46292(9) 0.0386(3) Uani 1 2 i d . . .
O4M O -0.03597(17) 0.32657(19) 0.39534(14) 0.0637(4) Uani 1 2 i d . . .
C1M C 0.3539(2) 0.55759(18) 0.27679(11) 0.0299(3) Uani 1 2 i d . . .
C2M C 0.2106(2) 0.6019(2) 0.27864(15) 0.0409(4) Uani 1 2 i d . . .
C3M C 0.1015(2) 0.5510(2) 0.33420(14) 0.0404(4) Uani 1 2 i d . . .
C4M C 0.1026(2) 0.43854(19) 0.40210(12) 0.0336(3) Uani 1 2 i d . . .
H2M H 0.206(3) 0.676(3) 0.2407(18) 0.057(6) Uiso 1 2 i d . . .
H3M H 0.018(3) 0.587(2) 0.3329(16) 0.047(5) Uiso 1 2 i 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'
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
_geom_angle_publ_flag
O1W Ni1 O1M 177.42(4) . . ?
O1W Ni1 O2W 88.78(5) . . ?
O1M Ni1 O2W 88.82(5) . . ?
O1W Ni1 N1 89.87(5) . . ?
O1M Ni1 N1 92.65(5) . . ?
O2W Ni1 N1 171.00(5) . . ?
O1W Ni1 N2 92.33(5) . . ?
O1M Ni1 N2 88.67(5) . . ?
O2W Ni1 N2 90.77(5) . . ?
N1 Ni1 N2 80.38(5) . . ?
O1W Ni1 O3W 87.75(5) . . ?
O1M Ni1 O3W 91.49(5) . . ?
O2W Ni1 O3W 94.84(5) . . ?
N1 Ni1 O3W 94.01(5) . . ?
N2 Ni1 O3W 174.39(5) . . ?
Ni1 O1W H11W 115.9(15) . . ?
Ni1 O1W H21W 118.9(17) . . ?
H11W O1W H21W 111(2) . . ?
Ni1 O2W H12W 114.6(14) . . ?
Ni1 O2W H22W 107.3(19) . . ?
H12W O2W H22W 110(2) . . ?
Ni1 O3W H13W 98.4(16) . . ?
Ni1 O3W H23W 110.9(17) . . ?
H13W O3W H23W 105(2) . . ?
H14W O4W H24W 118(2) . . ?
H14W O4W H35W 102(3) . . ?
H24W O4W H35W 116(2) . . ?
H15W O5W H25W 104(2) . . ?
H15W O5W H35W 101(3) . . ?
H25W O5W H35W 107(2) . . ?
C2 N1 C1 118.35(14) . . ?
C2 N1 Ni1 128.89(12) . . ?
C1 N1 Ni1 112.75(10) . . ?
C9 N2 C10 118.28(14) . . ?
C9 N2 Ni1 129.12(11) . . ?
C10 N2 Ni1 112.53(10) . . ?
N1 C1 C11 122.83(16) . . ?
N1 C1 C10 117.15(12) . . ?
C11 C1 C10 120.02(15) . . ?
N1 C2 C3 122.2(2) . . ?
N1 C2 H2 116.0(13) . . ?
C3 C2 H2 121.8(13) . . ?
C4 C3 C2 119.9(2) . . ?
C4 C3 H3 123.0(16) . . ?
C2 C3 H3 117.0(16) . . ?
C3 C4 C11 119.62(17) . . ?
C3 C4 H4 121.3(15) . . ?
C11 C4 H4 119.1(15) . . ?
C6 C5 C11 121.15(17) . . ?
C6 C5 H5 122.9(15) . . ?
C11 C5 H5 116.0(15) . . ?
C5 C6 C12 121.79(18) . . ?
C5 C6 H6 122.7(14) . . ?
C12 C6 H6 115.5(14) . . ?
C8 C7 C12 120.41(19) . . ?
C8 C7 H7 118.6(15) . . ?
C12 C7 H7 120.9(15) . . ?
C7 C8 C9 119.17(19) . . ?
C7 C8 H8 122.7(15) . . ?
C9 C8 H8 118.1(15) . . ?
N2 C9 C8 122.41(17) . . ?
N2 C9 H9 114.6(12) . . ?
C8 C9 H9 123.0(12) . . ?
N2 C10 C12 123.18(16) . . ?
N2 C10 C1 117.17(13) . . ?
C12 C10 C1 119.65(14) . . ?
C4 C11 C1 117.03(17) . . ?
C4 C11 C5 124.15(17) . . ?
C1 C11 C5 118.81(18) . . ?
C10 C12 C7 116.55(17) . . ?
C10 C12 C6 118.56(19) . . ?
C7 C12 C6 124.87(18) . . ?
C1M O1M Ni1 128.72(10) . . ?
O2M C1M O1M 125.77(14) . . ?
O2M C1M C2M 116.87(14) . . ?
O1M C1M C2M 117.35(14) . . ?
C3M C2M C1M 124.62(15) . . ?
C3M C2M H2M 120.0(14) . . ?
C1M C2M H2M 115.2(14) . . ?
C2M C3M C4M 124.37(15) . . ?
C2M C3M H3M 119.4(12) . . ?
C4M C3M H3M 116.2(12) . . ?
O4M C4M O3M 123.94(15) . . ?
O4M C4M C3M 117.20(15) . . ?
O3M C4M C3M 118.85(15) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1W 2.0503(11) . ?
Ni1 O1M 2.0604(10) . ?
Ni1 O2W 2.0679(11) . ?
Ni1 N1 2.0732(12) . ?
Ni1 N2 2.0767(13) . ?
Ni1 O3W 2.0830(12) . ?
O1W H11W 0.78(2) . ?
O1W H21W 0.88(3) . ?
O2W H12W 0.85(2) . ?
O2W H22W 0.81(3) . ?
O3W H13W 0.84(2) . ?
O3W H23W 0.85(3) . ?
O4W H14W 0.72(3) . ?
O4W H24W 1.3682(15) . ?
O4W H35W 1.42(6) . ?
O5W H15W 0.77(3) . ?
O5W H25W 1.3827(17) . ?
O5W H35W 1.37(6) . ?
N1 C2 1.319(2) . ?
N1 C1 1.354(2) . ?
N2 C9 1.325(2) . ?
N2 C10 1.3564(19) . ?
C1 C11 1.406(2) . ?
C1 C10 1.441(2) . ?
C2 C3 1.402(3) . ?
C2 H2 0.97(2) . ?
C3 C4 1.350(3) . ?
C3 H3 0.94(3) . ?
C4 C11 1.402(3) . ?
C4 H4 0.92(2) . ?
C5 C6 1.337(3) . ?
C5 C11 1.430(3) . ?
C5 H5 0.93(2) . ?
C6 C12 1.441(3) . ?
C6 H6 0.93(2) . ?
C7 C8 1.359(3) . ?
C7 C12 1.402(3) . ?
C7 H7 0.87(2) . ?
C8 C9 1.397(3) . ?
C8 H8 0.90(2) . ?
C9 H9 0.942(19) . ?
C10 C12 1.398(2) . ?
O1M C1M 1.2545(18) . ?
O2M C1M 1.246(2) . ?
O3M C4M 1.2604(19) . ?
O4M C4M 1.240(2) . ?
C1M C2M 1.496(2) . ?
C2M C3M 1.318(2) . ?
C2M H2M 0.93(2) . ?
C3M C4M 1.493(2) . ?
C3M H3M 0.93(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H11W O4M 0.78(2) 1.94(2) 2.685(2) 160(2) 1_655 yes
O1W H21W O4W 0.88(3) 1.81(3) 2.6852(19) 170(2) . yes
O2W H12W O3M 0.85(2) 1.92(2) 2.7622(16) 171(2) . yes
O2W H22W O3M 0.81(3) 1.96(3) 2.7299(19) 160(3) 2_666 yes
O3W H13W O2M 0.84(2) 1.81(3) 2.6282(17) 168(2) . yes
O3W H23W O3M 0.85(3) 1.96(3) 2.7576(17) 157(2) 2_666 yes
O4W H14W O2M 0.72(3) 2.06(3) 2.776(2) 175(3) 1_545 yes
O4W H24W O4W 1.3682(15) 1.3682(15) 2.736(3) 180.0 2_656 yes
O5W H15W O4M 0.77(3) 2.06(3) 2.794(2) 160(3) 1_655 yes
O5W H25W O5W 1.3827(17) 1.3827(17) 2.765(3) 180.0 2_756 yes
O5W H35W O4W 1.37(6) 1.42(6) 2.767(3) 167(4) . yes
