#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:27:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180340 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/09/7200979.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_7200979
loop_
_publ_author_name
'Walsh, David P.'
'Clérac, Rodolphe'
'Hearns, Nigel G. R.'
'Kruger, Paul E.'
'Schmitt, Wolfgang'
_publ_section_title
;
 Modulating topologies and magnetic properties of coordination polymers
 using 2,2′-bipyridine and 5-aminodiacetic isophthalic acid as
 ligands
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1666
_journal_paper_doi               10.1039/b902010a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C22 H29 N3 Ni2 O15'
_chemical_formula_weight         692.90
_chemical_name_systematic
;
?
;
_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                103.193(2)
_cell_angle_beta                 106.046(2)
_cell_angle_gamma                107.178(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0968(10)
_cell_length_b                   12.1101(12)
_cell_length_c                   12.5860(13)
_cell_measurement_reflns_used    207
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.67
_cell_volume                     1330.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14632
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0285
_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)+(0.0430P)²+0.5865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                4357
_reflns_number_total             4816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902010a.txt
_cod_data_source_block           dwni2b
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7200979
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.43490(3) 0.53857(2) 0.10136(2) 0.01234(9) Uani 1 1 d . . .
Ni2 Ni 0.18450(3) 0.85961(2) 0.65047(2) 0.01592(9) Uani 1 1 d . . .
O1 O 0.60639(15) 0.70232(13) 0.17692(12) 0.0165(3) Uani 1 1 d . . .
O2 O 0.83092(17) 0.80898(14) 0.31566(14) 0.0275(4) Uani 1 1 d . . .
O3 O 0.57645(15) 0.45516(13) 0.06281(12) 0.0150(3) Uani 1 1 d . . .
O4 O 0.71412(19) 0.35022(16) 0.11821(15) 0.0286(4) Uani 1 1 d . . .
O5 O 0.23355(18) 0.72726(14) 0.55688(15) 0.0275(4) Uani 1 1 d . . .
O8 O 0.13804(17) 0.17927(13) 0.31421(15) 0.0245(4) Uani 1 1 d . . .
O6 O 0.45334(18) 0.83412(14) 0.55556(15) 0.0279(4) Uani 1 1 d . . .
O11 O 0.37623(17) 1.00128(14) 0.66847(14) 0.0214(3) Uani 1 1 d D . .
O10 O 0.3055(2) 0.84381(17) 0.80200(16) 0.0379(4) Uani 1 1 d D . .
O12 O 0.0806(2) 0.88999(18) 0.50176(17) 0.0386(5) Uani 1 1 d D . .
O7 O -0.00275(17) 0.72012(13) 0.62837(15) 0.0236(4) Uani 1 1 d . . .
O13 O 0.13619(18) 0.99042(14) 0.75319(14) 0.0229(3) Uani 1 1 d D . .
C1 C 0.4484(2) 0.51085(19) 0.33577(17) 0.0140(4) Uani 1 1 d . . .
C2 C 0.4476(2) 0.61957(18) 0.40204(18) 0.0154(4) Uani 1 1 d . . .
H2 H 0.5184 0.6944 0.4118 0.019 Uiso 1 1 calc R . .
C3 C 0.3434(2) 0.40001(19) 0.32415(18) 0.0158(4) Uani 1 1 d . . .
H3 H 0.3459 0.3266 0.2836 0.019 Uiso 1 1 calc R . .
C4 C 0.3422(2) 0.61761(19) 0.45390(18) 0.0161(4) Uani 1 1 d . . .
C5 C 0.2343(2) 0.39750(19) 0.37264(18) 0.0158(4) Uani 1 1 d . . .
C6 C 0.2332(2) 0.50607(19) 0.43699(19) 0.0181(4) Uani 1 1 d . . .
H6 H 0.1601 0.5047 0.4688 0.022 Uiso 1 1 calc R . .
C7 C 0.3432(2) 0.73564(19) 0.52723(18) 0.0175(4) Uani 1 1 d . . .
C8 C 0.1163(2) 0.27640(19) 0.35140(18) 0.0175(4) Uani 1 1 d . . .
C9 C 0.6924(2) 0.62115(19) 0.32830(18) 0.0162(4) Uani 1 1 d . . .
H9A H 0.7716 0.5909 0.3303 0.019 Uiso 1 1 calc R . .
H9B H 0.7052 0.6600 0.4089 0.019 Uiso 1 1 calc R . .
C10 C 0.5730(2) 0.40145(19) 0.23133(18) 0.0165(4) Uani 1 1 d . . .
H10A H 0.4808 0.3308 0.2058 0.020 Uiso 1 1 calc R . .
H10B H 0.6462 0.3955 0.2961 0.020 Uiso 1 1 calc R . .
C11 C 0.7099(2) 0.71816(19) 0.26828(18) 0.0171(4) Uani 1 1 d . . .
C12 C 0.6288(2) 0.40097(18) 0.13006(18) 0.0156(4) Uani 1 1 d . . .
C13 C 0.2236(2) 0.26716(19) -0.00098(19) 0.0205(5) Uani 1 1 d . . .
H13 H 0.2969 0.2518 -0.0259 0.025 Uiso 1 1 calc R . .
C14 C 0.0976(3) 0.1683(2) -0.0179(2) 0.0265(5) Uani 1 1 d . . .
H14 H 0.0872 0.0882 -0.0528 0.032 Uiso 1 1 calc R . .
C15 C -0.0115(3) 0.1915(2) 0.0180(2) 0.0288(5) Uani 1 1 d . . .
H15 H -0.0966 0.1269 0.0081 0.035 Uiso 1 1 calc R . .
C16 C 0.0060(3) 0.3108(2) 0.0685(2) 0.0243(5) Uani 1 1 d . . .
H16 H -0.0674 0.3277 0.0922 0.029 Uiso 1 1 calc R . .
C17 C 0.1346(2) 0.4056(2) 0.08357(18) 0.0169(4) Uani 1 1 d . . .
C18 C 0.1634(2) 0.53698(19) 0.13711(18) 0.0174(4) Uani 1 1 d . . .
C19 C 0.0664(3) 0.5769(2) 0.1792(2) 0.0245(5) Uani 1 1 d . . .
H19 H -0.0226 0.5208 0.1745 0.029 Uiso 1 1 calc R . .
C20 C 0.1047(3) 0.7018(2) 0.2283(2) 0.0287(5) Uani 1 1 d . . .
H20 H 0.0423 0.7307 0.2584 0.034 Uiso 1 1 calc R . .
C21 C 0.2361(3) 0.7830(2) 0.2322(2) 0.0275(5) Uani 1 1 d . . .
H21 H 0.2630 0.8673 0.2641 0.033 Uiso 1 1 calc R . .
C22 C 0.3269(3) 0.7370(2) 0.1877(2) 0.0219(5) Uani 1 1 d . . .
H22 H 0.4147 0.7917 0.1892 0.026 Uiso 1 1 calc R . .
N1 N 0.54735(19) 0.51512(15) 0.27131(15) 0.0137(3) Uani 1 1 d . . .
N3 N 0.24330(19) 0.38373(16) 0.04991(15) 0.0158(4) Uani 1 1 d . . .
N2 N 0.29303(19) 0.61608(16) 0.14253(15) 0.0158(4) Uani 1 1 d . . .
O20 O 0.2804(2) 1.08212(17) 0.47110(17) 0.0322(4) Uani 1 1 d D . .
O22 O 0.3234(3) 1.1004(2) 1.2025(2) 0.0513(5) Uani 1 1 d D . .
O21 O 0.3710(5) 1.0476(4) 0.9876(5) 0.0515(11) Uani 0.50 1 d P . .
O21A O 0.3653(10) 0.9717(11) 1.0276(7) 0.057(3) Uani 0.25 1 d P . .
O21B O 0.9390(12) 0.5144(11) 0.3698(10) 0.070(3) Uani 0.25 1 d P . .
H13B H 0.043(2) 0.952(3) 0.732(4) 0.085 Uiso 1 1 d D . .
H11C H 0.416(4) 0.960(3) 0.629(3) 0.085 Uiso 1 1 d D . .
H11D H 0.351(4) 1.046(3) 0.628(3) 0.085 Uiso 1 1 d D . .
H12B H 0.129(4) 0.947(3) 0.482(4) 0.085 Uiso 1 1 d D . .
H12A H -0.006(3) 0.860(4) 0.446(3) 0.085 Uiso 1 1 d D . .
H13A H 0.135(4) 1.045(3) 0.723(3) 0.085 Uiso 1 1 d D . .
H22B H 0.253(4) 1.118(4) 1.227(4) 0.085 Uiso 1 1 d D . .
H10D H 0.320(5) 0.895(3) 0.867(2) 0.085 Uiso 1 1 d D . .
H10C H 0.294(5) 0.781(2) 0.824(3) 0.085 Uiso 1 1 d D . .
H22A H 0.410(3) 1.118(4) 1.256(3) 0.085 Uiso 1 1 d D . .
H20A H 0.363(2) 1.102(3) 0.459(3) 0.043(8) Uiso 1 1 d D . .
H20B H 0.228(3) 1.117(3) 0.435(3) 0.067(12) 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
O1 Ni1 N2 91.07(6) . . ?
O1 Ni1 O3 90.65(6) . 2_665 ?
N2 Ni1 O3 105.70(6) . 2_665 ?
O1 Ni1 N3 168.29(6) . . ?
N2 Ni1 N3 79.12(7) . . ?
O3 Ni1 N3 98.11(6) 2_665 . ?
O1 Ni1 O3 90.20(6) . . ?
N2 Ni1 O3 177.80(6) . . ?
O3 Ni1 O3 76.07(6) 2_665 . ?
N3 Ni1 O3 99.41(6) . . ?
O1 Ni1 N1 81.24(6) . . ?
N2 Ni1 N1 102.03(6) . . ?
O3 Ni1 N1 151.23(6) 2_665 . ?
N3 Ni1 N1 94.46(6) . . ?
O3 Ni1 N1 76.40(6) . . ?
O7 Ni2 O5 85.58(6) . . ?
O7 Ni2 O10 92.78(7) . . ?
O5 Ni2 O10 89.24(8) . . ?
O7 Ni2 O12 92.65(7) . . ?
O5 Ni2 O12 91.74(8) . . ?
O10 Ni2 O12 174.54(7) . . ?
O7 Ni2 O13 93.21(6) . . ?
O5 Ni2 O13 176.85(7) . . ?
O10 Ni2 O13 87.91(7) . . ?
O12 Ni2 O13 91.22(8) . . ?
O7 Ni2 O11 178.47(6) . . ?
O5 Ni2 O11 93.36(6) . . ?
O10 Ni2 O11 88.31(7) . . ?
O12 Ni2 O11 86.27(7) . . ?
O13 Ni2 O11 87.90(6) . . ?
C11 O1 Ni1 118.14(13) . . ?
C12 O3 Ni1 135.84(13) . 2_665 ?
C12 O3 Ni1 119.32(12) . . ?
Ni1 O3 Ni1 103.93(6) 2_665 . ?
C7 O5 Ni2 130.23(14) . . ?
C8 O7 Ni2 129.75(14) 2_566 . ?
C3 C1 C2 118.71(18) . . ?
C3 C1 N1 121.17(18) . . ?
C2 C1 N1 119.83(18) . . ?
C4 C2 C1 120.74(19) . . ?
C1 C3 C5 120.79(19) . . ?
C2 C4 C6 119.96(19) . . ?
C2 C4 C7 120.60(18) . . ?
C6 C4 C7 119.43(18) . . ?
C6 C5 C3 120.01(19) . . ?
C6 C5 C8 120.58(19) . . ?
C3 C5 C8 119.39(19) . . ?
C5 C6 C4 119.66(19) . . ?
O5 C7 O6 124.7(2) . . ?
O5 C7 C4 116.40(18) . . ?
O6 C7 C4 118.90(19) . . ?
O7 C8 O8 125.09(19) 2_566 . ?
O7 C8 C5 116.61(18) 2_566 . ?
O8 C8 C5 118.31(18) . . ?
N1 C9 C11 114.76(17) . . ?
N1 C10 C12 110.56(16) . . ?
O2 C11 O1 124.64(19) . . ?
O2 C11 C9 115.78(18) . . ?
O1 C11 C9 119.57(18) . . ?
O4 C12 O3 125.80(19) . . ?
O4 C12 C10 119.96(18) . . ?
O3 C12 C10 114.24(17) . . ?
N3 C13 C14 122.5(2) . . ?
C15 C14 C13 118.6(2) . . ?
C16 C15 C14 119.6(2) . . ?
C15 C16 C17 119.2(2) . . ?
N3 C17 C16 121.7(2) . . ?
N3 C17 C18 115.28(18) . . ?
C16 C17 C18 123.02(19) . . ?
N2 C18 C19 122.0(2) . . ?
N2 C18 C17 114.61(18) . . ?
C19 C18 C17 123.4(2) . . ?
C20 C19 C18 118.7(2) . . ?
C21 C20 C19 119.5(2) . . ?
C20 C21 C22 118.8(2) . . ?
N2 C22 C21 122.4(2) . . ?
C1 N1 C10 116.27(16) . . ?
C1 N1 C9 115.00(16) . . ?
C10 N1 C9 109.36(16) . . ?
C1 N1 Ni1 107.18(12) . . ?
C10 N1 Ni1 102.79(12) . . ?
C9 N1 Ni1 104.83(11) . . ?
C13 N3 C17 118.50(18) . . ?
C13 N3 Ni1 127.01(15) . . ?
C17 N3 Ni1 114.13(14) . . ?
C22 N2 C18 118.63(18) . . ?
C22 N2 Ni1 125.29(15) . . ?
C18 N2 Ni1 115.49(14) . . ?
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 O1 2.0089(14) . ?
Ni1 N2 2.0455(17) . ?
Ni1 O3 2.0578(14) 2_665 ?
Ni1 N3 2.0708(17) . ?
Ni1 O3 2.0762(14) . ?
Ni1 N1 2.2516(17) . ?
Ni2 O7 2.0282(15) . ?
Ni2 O5 2.0326(15) . ?
Ni2 O10 2.0454(18) . ?
Ni2 O12 2.0485(18) . ?
Ni2 O13 2.0709(16) . ?
Ni2 O11 2.0882(16) . ?
O1 C11 1.252(3) . ?
O2 C11 1.250(3) . ?
O3 C12 1.280(2) . ?
O3 Ni1 2.0578(14) 2_665 ?
O4 C12 1.218(3) . ?
O5 C7 1.247(3) . ?
O8 C8 1.269(3) . ?
O6 C7 1.260(3) . ?
O7 C8 1.251(3) 2_566 ?
C1 C3 1.389(3) . ?
C1 C2 1.392(3) . ?
C1 N1 1.448(3) . ?
C2 C4 1.391(3) . ?
C3 C5 1.396(3) . ?
C4 C6 1.394(3) . ?
C4 C7 1.510(3) . ?
C5 C6 1.383(3) . ?
C5 C8 1.502(3) . ?
C8 O7 1.251(3) 2_566 ?
C9 N1 1.482(3) . ?
C9 C11 1.529(3) . ?
C10 N1 1.477(3) . ?
C10 C12 1.528(3) . ?
C13 N3 1.339(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.378(4) . ?
C15 C16 1.375(3) . ?
C16 C17 1.387(3) . ?
C17 N3 1.353(3) . ?
C17 C18 1.482(3) . ?
C18 N2 1.347(3) . ?
C18 C19 1.387(3) . ?
C19 C20 1.384(3) . ?
C20 C21 1.379(4) . ?
C21 C22 1.381(3) . ?
C22 N2 1.342(3) . ?
O21 O21A 1.140(11) . ?
