#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:41:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179123 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308503.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_4308503
loop_
_publ_author_name
'Xin-Yi Wang'
'Hai-Yan Wei'
'Zhe-Ming Wang'
'Zhi-Da Chen'
'Song Gao'
_publ_section_title
;
Formate The Analogue of Azide: Structural and Magnetic Properties of
M(HCOO)2(4,4'-bpy).nH2O (M = Mn, Co, Ni; n= 0, 5)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              572
_journal_page_last               583
_journal_paper_doi               10.1021/ic049170t
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C12 H12 N2 Ni O5, 4(H2 O)'
_chemical_formula_sum            'C12 H20 N2 Ni O9'
_chemical_formula_weight         395.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 102.633(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4815(2)
_cell_length_b                   20.0601(4)
_cell_length_c                   8.1266(2)
_cell_measurement_reflns_used    10034
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1667.33(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski and Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) and maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15761
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.264(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3820
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0337P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                3245
_reflns_number_total             3820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049170tsi20040625_101613_4.cif
_cod_data_source_block           Ni-CHOO-Bpy-4-Ni
_cod_original_cell_volume        1667.33(6)
_cod_database_code               4308503
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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.94204(6) 0.253886(13) 0.51023(7) 0.01890(7) Uani 1 1 d . . .
O1 O 0.78412(18) 0.20359(7) 0.3619(2) 0.0273(4) Uani 1 1 d . . .
O2 O 0.60551(18) 0.19932(8) 0.1568(2) 0.0269(4) Uani 1 1 d . . .
O3 O 1.01202(17) 0.28371(8) 0.3018(2) 0.0282(4) Uani 1 1 d . . .
O4 O 1.0020(2) 0.28747(10) 0.0268(2) 0.0489(5) Uani 1 1 d . . .
O5 O 0.8828(2) 0.23164(9) 0.7305(2) 0.0325(4) Uani 1 1 d D . .
O6 O 0.7331(2) 0.13531(9) 0.8330(3) 0.0438(5) Uani 1 1 d D . .
O7 O 0.8438(3) 0.09199(11) 0.1538(3) 0.0518(6) Uani 1 1 d D . .
O8 O 0.6767(4) -0.01531(13) 0.1596(4) 0.0898(9) Uani 1 1 d D . .
O9 O 1.0458(4) 0.4228(2) 0.8733(6) 0.1030(13) Uani 1 1 d D . .
N1 N 0.8448(2) 0.34603(9) 0.5043(3) 0.0226(5) Uani 1 1 d . . .
N2 N 0.5369(2) 0.66150(9) 0.5181(3) 0.0248(5) Uani 1 1 d . . .
C1 C 0.8945(3) 0.40165(11) 0.4526(4) 0.0346(7) Uani 1 1 d . . .
H1 H 0.968(3) 0.3949(14) 0.400(4) 0.041 Uiso 1 1 d . . .
C2 C 0.7340(3) 0.35271(12) 0.5567(4) 0.0294(7) Uani 1 1 d . . .
H2 H 0.695(3) 0.3137(14) 0.585(4) 0.035 Uiso 1 1 d . . .
C3 C 0.8380(3) 0.46412(12) 0.4561(4) 0.0361(8) Uani 1 1 d . . .
H3 H 0.874(3) 0.4996(14) 0.394(4) 0.043 Uiso 1 1 d . . .
C4 C 0.6703(3) 0.41225(12) 0.5618(4) 0.0299(6) Uani 1 1 d . . .
H4 H 0.5926 0.4137 0.5992 0.036 Uiso 1 1 calc R . .
C5 C 0.7230(3) 0.47042(11) 0.5105(4) 0.0258(7) Uani 1 1 d . . .
C6 C 0.6596(3) 0.53653(11) 0.5163(3) 0.0249(7) Uani 1 1 d . . .
C7 C 0.7206(3) 0.59533(12) 0.4827(4) 0.0318(7) Uani 1 1 d . . .
H7 H 0.816(3) 0.5952(13) 0.472(3) 0.038 Uiso 1 1 d . . .
C8 C 0.5368(3) 0.54326(12) 0.5544(4) 0.0326(7) Uani 1 1 d . . .
H8 H 0.491(3) 0.5049(15) 0.582(3) 0.039 Uiso 1 1 d . . .
C9 C 0.6567(3) 0.65531(12) 0.4828(4) 0.0282(7) Uani 1 1 d . . .
H9 H 0.692(3) 0.6975(14) 0.445(4) 0.034 Uiso 1 1 d . . .
C10 C 0.4808(3) 0.60525(11) 0.5545(4) 0.0305(7) Uani 1 1 d . . .
H10 H 0.385(3) 0.6090(14) 0.575(4) 0.037 Uiso 1 1 d . . .
C11 C 0.6834(3) 0.22880(9) 0.2724(4) 0.0239(5) Uani 1 1 d . . .
H11 H 0.661(2) 0.2797(11) 0.291(3) 0.029 Uiso 1 1 d . . .
C12 C 0.9744(3) 0.26363(14) 0.1525(4) 0.0335(7) Uani 1 1 d . . .
H12 H 0.918(3) 0.2196(16) 0.148(4) 0.040 Uiso 1 1 d . . .
H7WA H 0.835(4) 0.1171(18) 0.253(4) 0.109(16) Uiso 1 1 d D . .
H9WA H 1.056(7) 0.3769(11) 0.878(8) 0.18(3) Uiso 1 1 d D . .
H9WB H 1.083(5) 0.438(2) 0.782(5) 0.14(3) Uiso 1 1 d D . .
H7WB H 0.780(3) 0.0582(15) 0.159(5) 0.082(13) Uiso 1 1 d D . .
H8WA H 0.709(6) -0.055(2) 0.221(7) 0.15(2) Uiso 1 1 d D . .
H5WA H 0.924(3) 0.2490(13) 0.838(3) 0.051(14) Uiso 1 1 d D . .
H6WA H 0.656(3) 0.1596(19) 0.826(5) 0.106(16) Uiso 1 1 d D . .
H6WB H 0.776(3) 0.131(2) 0.946(3) 0.089(13) Uiso 1 1 d D . .
H5WB H 0.830(3) 0.1966(12) 0.745(4) 0.062(11) Uiso 1 1 d D . .
H8WB H 0.657(17) -0.029(4) 0.044(3) 0.47(10) Uiso 1 1 d 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
O5 Ni1 O3 174.44(8) . . ?
O5 Ni1 O1 92.61(8) . . ?
O3 Ni1 O1 92.59(8) . . ?
O5 Ni1 O2 88.13(8) . 4 ?
O3 Ni1 O2 86.76(8) . 4 ?
O1 Ni1 O2 177.41(9) . 4 ?
O5 Ni1 N2 90.74(9) . 3_545 ?
O3 Ni1 N2 91.71(8) . 3_545 ?
O1 Ni1 N2 84.34(8) . 3_545 ?
O2 Ni1 N2 93.17(8) 4 3_545 ?
O5 Ni1 N1 88.50(8) . . ?
O3 Ni1 N1 89.08(8) . . ?
O1 Ni1 N1 95.32(8) . . ?
O2 Ni1 N1 87.18(8) 4 . ?
N2 Ni1 N1 179.15(12) 3_545 . ?
C11 O1 Ni1 127.14(14) . . ?
C11 O2 Ni1 122.44(15) . 4_454 ?
C12 O3 Ni1 127.1(2) . . ?
C2 N1 C1 116.4(2) . . ?
C2 N1 Ni1 122.26(16) . . ?
C1 N1 Ni1 121.3(2) . . ?
C10 N2 C9 116.3(2) . . ?
C10 N2 Ni1 121.64(19) . 3_455 ?
C9 N2 Ni1 122.03(16) . 3_455 ?
N1 C1 C3 123.3(3) . . ?
N1 C2 C4 124.2(2) . . ?
C5 C3 C1 119.7(3) . . ?
C2 C4 C5 119.5(3) . . ?
C3 C5 C4 116.8(2) . . ?
C3 C5 C6 121.3(2) . . ?
C4 C5 C6 121.9(2) . . ?
C8 C6 C7 116.5(2) . . ?
C8 C6 C5 122.20(19) . . ?
C7 C6 C5 121.3(2) . . ?
C9 C7 C6 119.6(3) . . ?
C10 C8 C6 120.2(2) . . ?
N2 C9 C7 123.7(2) . . ?
N2 C10 C8 123.7(3) . . ?
O2 C11 O1 125.10(18) . . ?
O4 C12 O3 127.0(3) . . ?
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 O5 2.0677(19) . ?
Ni1 O3 2.0754(19) . ?
Ni1 O1 2.083(2) . ?
Ni1 O2 2.0840(19) 4 ?
Ni1 N2 2.098(2) 3_545 ?
Ni1 N1 2.106(2) . ?
O1 C11 1.250(3) . ?
O2 C11 1.250(3) . ?
O2 Ni1 2.0840(19) 4_454 ?
O3 C12 1.257(3) . ?
O4 C12 1.219(4) . ?
N1 C2 1.328(4) . ?
N1 C1 1.337(3) . ?
N2 C10 1.335(3) . ?
N2 C9 1.353(4) . ?
N2 Ni1 2.098(2) 3_455 ?
C1 C3 1.389(4) . ?
C2 C4 1.373(4) . ?
C3 C5 1.378(4) . ?
C4 C5 1.393(4) . ?
C5 C6 1.489(2) . ?
C6 C8 1.395(4) . ?
C6 C7 1.397(4) . ?
C7 C9 1.377(4) . ?
C8 C10 1.375(4) . ?
