#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:24:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179109 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/71/4307172.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_4307172
loop_
_publ_author_name
'A. K. Ghosh'
'D. Ghoshal'
'E. Zangrando'
'J. Ribas'
'N. Ray Chaudhuri'
_publ_section_title
;
Syntheses, Crystal Structures, and Magnetic Properties of Metal-Organic
Hybrid Materials of Cu(II): Effect of a Long Chain Dicarboxylate
Backbone, and Counteranion in Their Structural Diversity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3057
_journal_page_last               3071
_journal_paper_doi               10.1021/ic061720v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C30 H32 Cu2 N4 O10, 2(H3 B O3), 4(H2 O)'
_chemical_formula_sum            'C30 H46 B2 Cu2 N4 O20'
_chemical_formula_weight         931.41
_chemical_name_systematic
;
 bis[mu2-glutarato,O,O'-aquo-(2,2'bipyridine)-copper(II)] 
 bis(orthoboric acid) tetrahydrated
;
_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                101.13(2)
_cell_angle_beta                 94.29(2)
_cell_angle_gamma                111.49(2)
_cell_formula_units_Z            1
_cell_length_a                   8.748(2)
_cell_length_b                   10.528(2)
_cell_length_c                   12.232(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1015.4(4)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Xpress'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.70.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0363
_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       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12195
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.7738
_exptl_absorpt_correction_T_min  0.6771
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5207
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0381
_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)+(0.0706P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                4182
_reflns_number_total             5207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061720vsi20060911_023753_1.cif
_cod_data_source_block           ind438complex1
_cod_database_code               4307172
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
Cu Cu 0.62484(3) 0.86708(2) 0.235831(18) 0.04814(9) Uani 1 1 d D . .
O1W O 0.8604(2) 1.02811(16) 0.17936(14) 0.0654(4) Uani 1 1 d D . .
H11 H 0.928(3) 0.984(3) 0.162(3) 0.098 Uiso 1 1 d D . .
H12 H 0.864(4) 1.066(3) 0.124(2) 0.098 Uiso 1 1 d D . .
N1 N 0.5158(2) 1.00248(17) 0.22872(14) 0.0516(3) Uani 1 1 d . . .
N2 N 0.6987(2) 0.98014(16) 0.39621(13) 0.0481(3) Uani 1 1 d . . .
C1 C 0.4225(3) 1.0042(2) 0.13717(19) 0.0632(5) Uani 1 1 d . . .
H1 H 0.3911 0.9299 0.0737 0.076 Uiso 1 1 calc R . .
C2 C 0.3723(3) 1.1137(3) 0.1352(2) 0.0727(6) Uani 1 1 d . . .
H2 H 0.3064 1.1128 0.0715 0.087 Uiso 1 1 calc R . .
C3 C 0.4203(3) 1.2234(3) 0.2278(2) 0.0697(6) Uani 1 1 d . . .
H3 H 0.3892 1.2989 0.2270 0.084 Uiso 1 1 calc R . .
C4 C 0.5151(3) 1.2219(2) 0.3225(2) 0.0650(5) Uani 1 1 d . . .
H4 H 0.5480 1.2956 0.3864 0.078 Uiso 1 1 calc R . .
C5 C 0.5605(2) 1.1089(2) 0.32082(17) 0.0520(4) Uani 1 1 d . . .
C6 C 0.6569(2) 1.09270(19) 0.41853(16) 0.0499(4) Uani 1 1 d . . .
C7 C 0.6981(3) 1.1810(2) 0.52554(18) 0.0602(5) Uani 1 1 d . . .
H7 H 0.6699 1.2590 0.5393 0.072 Uiso 1 1 calc R . .
C8 C 0.7814(3) 1.1519(2) 0.61097(18) 0.0629(5) Uani 1 1 d . . .
H8 H 0.8091 1.2095 0.6834 0.075 Uiso 1 1 calc R . .
C9 C 0.8237(3) 1.0359(2) 0.58825(18) 0.0603(5) Uani 1 1 d . . .
H9 H 0.8801 1.0147 0.6450 0.072 Uiso 1 1 calc R . .
C10 C 0.7804(3) 0.9526(2) 0.47996(16) 0.0543(4) Uani 1 1 d . . .
H10 H 0.8088 0.8748 0.4644 0.065 Uiso 1 1 calc R . .
O1 O 0.74284(18) 0.74456(14) 0.25460(11) 0.0534(3) Uani 1 1 d . . .
O2 O 0.9308(2) 0.79973(17) 0.14096(15) 0.0691(4) Uani 1 1 d . . .
O3 O 0.49989(18) 0.73702(14) 0.09162(11) 0.0544(3) Uani 1 1 d . . .
O4 O 0.34997(19) 0.63846(15) 0.21318(12) 0.0612(4) Uani 1 1 d . . .
C11 C 0.8455(2) 0.7180(2) 0.19394(16) 0.0512(4) Uani 1 1 d . . .
C12 C 0.8562(3) 0.5767(2) 0.18806(17) 0.0562(5) Uani 1 1 d . . .
H12A H 0.8478 0.5547 0.2614 0.067 Uiso 1 1 calc R . .
H12B H 0.9632 0.5808 0.1688 0.067 Uiso 1 1 calc R . .
C13 C 0.7170(3) 0.4614(2) 0.09986(16) 0.0532(4) Uani 1 1 d . . .
H13A H 0.7184 0.3707 0.1041 0.064 Uiso 1 1 calc R . .
H13B H 0.6105 0.4617 0.1168 0.064 Uiso 1 1 calc R . .
C14 C 0.2659(3) 0.5196(2) 0.01904(16) 0.0552(4) Uani 1 1 d . . .
H14A H 0.1517 0.5018 0.0295 0.066 Uiso 1 1 calc R . .
H14B H 0.2856 0.4362 0.0252 0.066 Uiso 1 1 calc R . .
C15 C 0.3787(2) 0.63957(19) 0.11452(16) 0.0502(4) Uani 1 1 d . . .
B1 B 0.1444(3) 0.3684(2) 0.3446(2) 0.0573(5) Uani 1 1 d . . .
O5 O 0.1181(2) 0.39713(17) 0.24389(14) 0.0637(4) Uani 1 1 d D . .
H51 H 0.184(3) 0.466(2) 0.235(2) 0.076 Uiso 1 1 d D . .
O6 O 0.2643(2) 0.47051(17) 0.42805(14) 0.0673(4) Uani 1 1 d D . .
H61 H 0.283(4) 0.438(3) 0.4822(19) 0.081 Uiso 1 1 d D . .
O7 O 0.0577(2) 0.24160(17) 0.36588(15) 0.0718(4) Uani 1 1 d D . .
H71 H -0.011(3) 0.193(3) 0.313(2) 0.086 Uiso 1 1 d D . .
O2W O 0.5967(3) 0.5767(2) 0.39336(18) 0.0856(6) Uani 1 1 d D . .
H21 H 0.640(4) 0.636(3) 0.359(3) 0.128 Uiso 1 1 d D . .
H22 H 0.496(2) 0.566(4) 0.392(3) 0.128 Uiso 1 1 d D . .
O3W O -0.0966(2) 0.21388(19) 0.04472(15) 0.0702(4) Uani 1 1 d D . .
H31 H -0.033(4) 0.277(3) 0.1019(19) 0.105 Uiso 1 1 d D . .
H32 H -0.044(4) 0.216(4) -0.0087(19) 0.105 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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 Cu O3 89.84(6) . . ?
O1 Cu N1 175.27(6) . . ?
O3 Cu N1 94.89(7) . . ?
O1 Cu N2 94.24(6) . . ?
O3 Cu N2 165.90(6) . . ?
N1 Cu N2 81.19(7) . . ?
O1 Cu O1W 91.41(6) . . ?
O3 Cu O1W 102.70(6) . . ?
N1 Cu O1W 87.47(7) . . ?
N2 Cu O1W 90.70(7) . . ?
C1 N1 C5 119.53(18) . . ?
C1 N1 Cu 125.54(15) . . ?
C5 N1 Cu 114.36(14) . . ?
C10 N2 C6 119.07(16) . . ?
C10 N2 Cu 126.53(13) . . ?
C6 N2 Cu 114.40(13) . . ?
N1 C1 C2 121.4(2) . . ?
C3 C2 C1 119.3(2) . . ?
C2 C3 C4 119.6(2) . . ?
C3 C4 C5 118.9(2) . . ?
N1 C5 C4 121.2(2) . . ?
N1 C5 C6 114.81(17) . . ?
C4 C5 C6 123.95(18) . . ?
N2 C6 C7 121.45(18) . . ?
N2 C6 C5 114.24(16) . . ?
C7 C6 C5 124.28(18) . . ?
C8 C7 C6 119.13(19) . . ?
C7 C8 C9 119.46(18) . . ?
C10 C9 C8 118.7(2) . . ?
N2 C10 C9 122.15(19) . . ?
C11 O1 Cu 127.23(13) . . ?
C15 O3 Cu 107.11(12) . . ?
O2 C11 O1 123.57(19) . . ?
O2 C11 C12 120.53(18) . . ?
O1 C11 C12 115.90(18) . . ?
C11 C12 C13 110.83(16) . . ?
C14 C13 C12 112.27(18) 2_665 . ?
C15 C14 C13 116.87(17) . 2_665 ?
O4 C15 O3 122.64(18) . . ?
O4 C15 C14 118.72(18) . . ?
O3 C15 C14 118.63(17) . . ?
O5 B1 O7 122.2(2) . . ?
O5 B1 O6 118.7(2) . . ?
O7 B1 O6 119.0(2) . . ?
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
Cu O1 1.9587(14) . ?
Cu O3 1.9657(15) . ?
Cu N1 1.9952(17) . ?
Cu N2 2.0070(16) . ?
Cu O1W 2.3880(17) . ?
N1 C1 1.342(3) . ?
N1 C5 1.343(3) . ?
N2 C10 1.342(3) . ?
N2 C6 1.349(2) . ?
C1 C2 1.380(3) . ?
C2 C3 1.364(4) . ?
C3 C4 1.380(4) . ?
C4 C5 1.382(3) . ?
C5 C6 1.484(3) . ?
C6 C7 1.386(3) . ?
C7 C8 1.375(3) . ?
C8 C9 1.385(3) . ?
C9 C10 1.379(3) . ?
O1 C11 1.280(2) . ?
O2 C11 1.239(3) . ?
O3 C15 1.270(2) . ?
O4 C15 1.252(2) . ?
C11 C12 1.512(3) . ?
C12 C13 1.529(3) . ?
C13 C14 1.517(3) 2_665 ?
C14 C15 1.509(3) . ?
C14 C13 1.517(3) 2_665 ?
B1 O5 1.346(3) . ?
B1 O7 1.359(3) . ?
B1 O6 1.374(3) . ?
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
O1W H11 O2 0.896(16) 1.91(2) 2.660(2) 139.9(18) .
O1W H12 O3W 0.844(17) 1.933(19) 2.734(3) 158(3) 1_665
O5 H51 O4 0.775(17) 1.949(17) 2.724(2) 179(3) .
O6 H61 O2W 0.836(17) 1.85(2) 2.638(2) 157(3) 2_666
O7 H71 O1W 0.799(17) 2.03(2) 2.797(3) 160(3) 1_445
O2W H21 O1 0.815(18) 1.929(19) 2.732(2) 168(4) .
O2W H22 O6 0.847(18) 2.03(2) 2.805(3) 152(3) .
O3W H31 O5 0.855(17) 1.986(18) 2.834(3) 171(4) .
O3W H32 O2 0.828(17) 1.968(17) 2.793(2) 174(3) 2_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Cu N1 C1 165.6(7) . . . . ?
O3 Cu N1 C1 -13.26(19) . . . . ?
N2 Cu N1 C1 -179.61(19) . . . . ?
O1W Cu N1 C1 89.28(19) . . . . ?
O1 Cu N1 C5 -5.6(8) . . . . ?
O3 Cu N1 C5 175.48(14) . . . . ?
N2 Cu N1 C5 9.13(14) . . . . ?
O1W Cu N1 C5 -81.98(14) . . . . ?
O1 Cu N2 C10 -7.97(17) . . . . ?
O3 Cu N2 C10 98.5(3) . . . . ?
N1 Cu N2 C10 173.24(18) . . . . ?
O1W Cu N2 C10 -99.44(17) . . . . ?
O1 Cu N2 C6 173.15(13) . . . . ?
O3 Cu N2 C6 -80.4(3) . . . . ?
N1 Cu N2 C6 -5.65(13) . . . . ?
O1W Cu N2 C6 81.68(14) . . . . ?
C5 N1 C1 C2 0.5(3) . . . . ?
Cu N1 C1 C2 -170.36(18) . . . . ?
N1 C1 C2 C3 0.8(4) . . . . ?
C1 C2 C3 C4 -1.3(4) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C1 N1 C5 C4 -1.3(3) . . . . ?
Cu N1 C5 C4 170.50(17) . . . . ?
C1 N1 C5 C6 177.34(19) . . . . ?
Cu N1 C5 C6 -10.8(2) . . . . ?
C3 C4 C5 N1 0.8(3) . . . . ?
C3 C4 C5 C6 -177.7(2) . . . . ?
C10 N2 C6 C7 0.7(3) . . . . ?
Cu N2 C6 C7 179.66(16) . . . . ?
C10 N2 C6 C5 -177.43(17) . . . . ?
Cu N2 C6 C5 1.5(2) . . . . ?
N1 C5 C6 N2 6.1(3) . . . . ?
C4 C5 C6 N2 -175.23(19) . . . . ?
N1 C5 C6 C7 -171.92(18) . . . . ?
C4 C5 C6 C7 6.7(3) . . . . ?
N2 C6 C7 C8 -0.9(3) . . . . ?
C5 C6 C7 C8 177.0(2) . . . . ?
C6 C7 C8 C9 0.6(3) . . . . ?
C7 C8 C9 C10 -0.1(3) . . . . ?
C6 N2 C10 C9 -0.2(3) . . . . ?
Cu N2 C10 C9 -179.00(16) . . . . ?
C8 C9 C10 N2 -0.1(3) . . . . ?
O3 Cu O1 C11 66.13(16) . . . . ?
N1 Cu O1 C11 -112.8(7) . . . . ?
N2 Cu O1 C11 -127.39(16) . . . . ?
O1W Cu O1 C11 -36.58(16) . . . . ?
O1 Cu O3 C15 83.00(14) . . . . ?
N1 Cu O3 C15 -97.09(14) . . . . ?
N2 Cu O3 C15 -24.0(3) . . . . ?
O1W Cu O3 C15 174.41(13) . . . . ?
Cu O1 C11 O2 26.9(3) . . . . ?
Cu O1 C11 C12 -152.05(13) . . . . ?
O2 C11 C12 C13 -96.4(2) . . . . ?
O1 C11 C12 C13 82.6(2) . . . . ?
C11 C12 C13 C14 65.7(2) . . . 2_665 ?
Cu O3 C15 O4 2.6(2) . . . . ?
Cu O3 C15 C14 -176.74(15) . . . . ?
C13 C14 C15 O4 168.13(19) 2_665 . . . ?
C13 C14 C15 O3 -12.5(3) 2_665 . . . ?
C11 C12 C13 C14 65.7(2) . . . 2_665 ?
C12 C13 C14 C15 169.96(17) . . 2_665 2_665 ?
