#------------------------------------------------------------------------------
#$Date: 2015-07-08 06:59:39 +0300 (Wed, 08 Jul 2015) $
#$Revision: 140988 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/09/2240904.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_2240904
loop_
_publ_author_name
'Granifo, Juan'
'Suarez, Sebastián'
'Baggio, Ricardo'
_publ_section_title
;
 Structure of a dinuclear cadmium complex with 2,2'-bipyridine,
 monodentate nitrate and 3-carboxy-6-methylpyridine-2-carboxylate ligands:
 intramolecular carbonyl(lone pair)···π(ring) and
 nitrate(π)···π(ring) interactions.
;
_journal_coeditor_code           SJ5468
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              890
_journal_page_last               894
_journal_paper_doi               10.1107/S2056989015012384
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Cd2 (C8 H6 N O4)2 (N O3)2 (C10 H8 N2)2], C H4 O'
_chemical_formula_moiety         'C36 H28 Cd2 N8 O14, C H4 O'
_chemical_formula_sum            'C37 H32 Cd2 N8 O15'
_chemical_formula_weight         1053.50
_chemical_name_systematic
;Bis(μ-3-carboxy-6-methylpyridine-2-carboxylato)-κ³N,O²:O²;κ³O²:N,O²-bis[(2,2'-bipyridine-κ²N,N'))(nitrato-κO)cadmium]
methanol monosolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                71.241(4)
_cell_angle_beta                 86.537(4)
_cell_angle_gamma                86.803(5)
_cell_formula_units_Z            1
_cell_length_a                   8.4096(5)
_cell_length_b                   10.9626(6)
_cell_length_c                   11.5056(4)
_cell_measurement_reflns_used    2675
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.84
_cell_measurement_theta_min      3.76
_cell_volume                     1001.79(9)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD S Ultra'
_diffrn_measurement_method       'ω scans, thick slices'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            21744
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.082
_diffrn_reflns_theta_min         3.630
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.739
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0394P)²+1.5425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                4155
_reflns_number_total             4819
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            sj5468sup1.cf
_cod_data_source_block           I
_cod_database_code               2240904
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_occupancy
Cd Cd1 0.47993(3) 0.63548(2) 0.35527(2) 0.01961(9) Uani d 1
N N1A 0.6981(3) 0.7364(3) 0.3922(3) 0.0229(6) Uani d 1
N N2A 0.4198(3) 0.8540(3) 0.3047(2) 0.0223(6) Uani d 1
C C1A 0.8378(4) 0.6740(4) 0.4272(3) 0.0279(7) Uani d 1
H H1A 0.8516 0.5882 0.4306 0.033 Uiso calc 1
C C2A 0.9614(4) 0.7331(4) 0.4581(3) 0.0292(8) Uani d 1
H H2A 1.0575 0.6883 0.4821 0.035 Uiso calc 1
C C3A 0.9393(4) 0.8601(4) 0.4526(3) 0.0312(8) Uani d 1
H H3A 1.0204 0.9020 0.4740 0.037 Uiso calc 1
C C4A 0.7968(4) 0.9252(4) 0.4152(3) 0.0286(7) Uani d 1
H H4A 0.7812 1.0114 0.4104 0.034 Uiso calc 1
C C5A 0.6771(4) 0.8603(3) 0.3851(3) 0.0196(6) Uani d 1
C C6A 0.5211(4) 0.9244(3) 0.3409(3) 0.0201(6) Uani d 1
C C7A 0.4801(4) 1.0501(3) 0.3369(3) 0.0263(7) Uani d 1
H H7A 0.5504 1.0976 0.3629 0.032 Uiso calc 1
C C8A 0.3343(4) 1.1041(3) 0.2940(3) 0.0286(8) Uani d 1
H H8A 0.3048 1.1877 0.2920 0.034 Uiso calc 1
C C9A 0.2327(4) 1.0328(3) 0.2540(3) 0.0303(8) Uani d 1
H H9A 0.1348 1.0679 0.2230 0.036 Uiso calc 1
C C10A 0.2801(4) 0.9084(3) 0.2614(3) 0.0280(7) Uani d 1
H H10A 0.2116 0.8599 0.2351 0.034 Uiso calc 1
O O1B 0.6097(3) 0.4384(2) 0.44192(19) 0.0216(5) Uani d 1
O O2B 0.7028(3) 0.2598(2) 0.4031(2) 0.0256(5) Uani d 1
O O3B 0.8147(3) 0.1816(3) 0.1644(3) 0.0390(6) Uani d 1
O O4B 0.9923(3) 0.2717(3) 0.2400(3) 0.0340(6) Uani d 1
H H4BO 1.004(6) 0.344(2) 0.248(4) 0.051(14) Uiso d 1
N N1B 0.5964(3) 0.5661(3) 0.1972(2) 0.0200(5) Uani d 1
C C1B 0.6745(4) 0.4503(3) 0.2349(3) 0.0185(6) Uani d 1
C C2B 0.7605(4) 0.3994(3) 0.1523(3) 0.0226(7) Uani d 1
C C3B 0.7607(5) 0.4714(4) 0.0288(3) 0.0316(8) Uani d 1
H H3B 0.8164 0.4402 -0.0288 0.038 Uiso calc 1
C C4B 0.6796(5) 0.5880(4) -0.0090(3) 0.0343(9) Uani d 1
H H4B 0.6799 0.6361 -0.0919 0.041 Uiso calc 1
C C5B 0.5963(4) 0.6345(3) 0.0780(3) 0.0255(7) Uani d 1
C C6B 0.6608(4) 0.3736(3) 0.3714(3) 0.0185(6) Uani d 1
C C7B 0.8543(4) 0.2739(3) 0.1893(3) 0.0265(7) Uani d 1
C C8B 0.5036(5) 0.7606(4) 0.0418(3) 0.0376(9) Uani d 1
H H8BA 0.5131 0.7999 -0.0457 0.056 Uiso calc 1
H H8BB 0.3934 0.7462 0.0669 0.056 Uiso calc 1
H H8BC 0.5448 0.8166 0.0811 0.056 Uiso calc 1
N N1C 0.1872(3) 0.5118(3) 0.2872(2) 0.0248(6) Uani d 1
O O1C 0.2228(3) 0.6168(3) 0.3000(3) 0.0350(6) Uani d 1
O O2C 0.2871(3) 0.4227(3) 0.2993(3) 0.0341(6) Uani d 1
O O3C 0.0460(3) 0.5009(3) 0.2619(3) 0.0374(6) Uani d 1
O O1M 0.7710(10) 0.9624(9) 0.0748(8) 0.072(2) Uani d 0.5
H H1M 0.816(4) 1.0346(13) 0.046(17) 0.18(9) Uiso d 0.5
C C1M 0.8993(11) 0.8676(10) 0.0932(8) 0.060(3) Uani d 0.5
H H1M1 0.9936 0.9068 0.0490 0.090 Uiso calc 0.5
H H1M2 0.8713 0.7994 0.0637 0.090 Uiso calc 0.5
H H1M3 0.9189 0.8331 0.1792 0.090 Uiso calc 0.5
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'
Cd Cd -0.8075 1.2024 '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
O1B Cd1 O1B 2_666 . 73.38(8)
O1B Cd1 N2A 2_666 . 101.83(9)
O1B Cd1 N2A . . 159.48(9)
O1B Cd1 N1A 2_666 . 94.90(9)
O1B Cd1 N1A . . 89.17(9)
N2A Cd1 N1A . . 71.15(10)
O1B Cd1 O1C 2_666 . 88.36(9)
O1B Cd1 O1C . . 112.97(9)
N2A Cd1 O1C . . 86.44(9)
N1A Cd1 O1C . . 157.56(10)
O1B Cd1 N1B 2_666 . 142.36(8)
O1B Cd1 N1B . . 71.66(8)
N2A Cd1 N1B . . 115.79(9)
N1A Cd1 N1B . . 98.09(9)
O1C Cd1 N1B . . 92.65(9)
C5A N1A C1A . . 119.8(3)
C5A N1A Cd1 . . 117.1(2)
C1A N1A Cd1 . . 123.0(2)
C10A N2A C6A . . 118.9(3)
C10A N2A Cd1 . . 123.4(2)
C6A N2A Cd1 . . 116.7(2)
N1A C1A C2A . . 122.1(3)
N1A C1A H1A . . 119.0
C2A C1A H1A . . 119.0
C3A C2A C1A . . 118.3(3)
C3A C2A H2A . . 120.9
C1A C2A H2A . . 120.9
C2A C3A C4A . . 119.9(3)
C2A C3A H3A . . 120.0
C4A C3A H3A . . 120.0
C3A C4A C5A . . 118.9(3)
C3A C4A H4A . . 120.5
C5A C4A H4A . . 120.5
N1A C5A C4A . . 121.0(3)
N1A C5A C6A . . 116.7(3)
C4A C5A C6A . . 122.3(3)
N2A C6A C7A . . 121.0(3)
N2A C6A C5A . . 116.6(3)
C7A C6A C5A . . 122.4(3)
C8A C7A C6A . . 119.4(3)
C8A C7A H7A . . 120.3
C6A C7A H7A . . 120.3
C7A C8A C9A . . 119.4(3)
C7A C8A H8A . . 120.3
C9A C8A H8A . . 120.3
C10A C9A C8A . . 118.2(3)
C10A C9A H9A . . 120.9
C8A C9A H9A . . 120.9
N2A C10A C9A . . 123.1(3)
N2A C10A H10A . . 118.4
C9A C10A H10A . . 118.4
C6B O1B Cd1 . 2_666 128.9(2)
C6B O1B Cd1 . . 118.42(19)
Cd1 O1B Cd1 2_666 . 106.62(8)
C7B O4B H4BO . . 109(3)
C5B N1B C1B . . 120.4(3)
C5B N1B Cd1 . . 124.9(2)
C1B N1B Cd1 . . 114.7(2)
N1B C1B C2B . . 121.7(3)
N1B C1B C6B . . 117.5(3)
C2B C1B C6B . . 120.7(3)
C3B C2B C1B . . 117.6(3)
C3B C2B C7B . . 118.4(3)
C1B C2B C7B . . 124.1(3)
C4B C3B C2B . . 120.4(3)
C4B C3B H3B . . 119.8
C2B C3B H3B . . 119.8
C3B C4B C5B . . 119.6(3)
C3B C4B H4B . . 120.2
C5B C4B H4B . . 120.2
N1B C5B C4B . . 120.4(3)
N1B C5B C8B . . 117.7(3)
C4B C5B C8B . . 121.9(3)
O2B C6B O1B . . 126.7(3)
O2B C6B C1B . . 118.0(3)
O1B C6B C1B . . 115.3(3)
O3B C7B O4B . . 120.6(3)
O3B C7B C2B . . 122.0(3)
O4B C7B C2B . . 117.1(3)
C5B C8B H8BA . . 109.5
C5B C8B H8BB . . 109.5
H8BA C8B H8BB . . 109.5
C5B C8B H8BC . . 109.5
H8BA C8B H8BC . . 109.5
H8BB C8B H8BC . . 109.5
O2C N1C O3C . . 121.1(3)
O2C N1C O1C . . 121.0(3)
O3C N1C O1C . . 117.9(3)
N1C O1C Cd1 . . 118.4(2)
C1M O1M H1M . . 104.7(13)
O1M C1M H1M1 . . 109.5
O1M C1M H1M2 . . 109.5
H1M1 C1M H1M2 . . 109.5
O1M C1M H1M3 . . 109.5
H1M1 C1M H1M3 . . 109.5
H1M2 C1M H1M3 . . 109.5
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
Cd1 O1B 2_666 2.304(2) y
Cd1 O1B . 2.310(2) y
Cd1 N2A . 2.310(3) y
Cd1 N1A . 2.323(3) y
Cd1 O1C . 2.329(2) y
Cd1 N1B . 2.332(3) y
N1A C5A . 1.336(4) ?
N1A C1A . 1.342(4) ?
N2A C10A . 1.336(4) ?
N2A C6A . 1.349(4) ?
C1A C2A . 1.377(5) ?
C1A H1A . 0.9300 ?
C2A C3A . 1.375(5) ?
C2A H2A . 0.9300 ?
C3A C4A . 1.378(5) ?
C3A H3A . 0.9300 ?
C4A C5A . 1.387(5) ?
C4A H4A . 0.9300 ?
C5A C6A . 1.490(4) ?
C6A C7A . 1.389(5) ?
C7A C8A . 1.379(5) ?
C7A H7A . 0.9300 ?
C8A C9A . 1.380(5) ?
C8A H8A . 0.9300 ?
C9A C10A . 1.377(5) ?
C9A H9A . 0.9300 ?
C10A H10A . 0.9300 ?
O1B C6B . 1.281(4) ?
O2B C6B . 1.220(4) ?
O3B C7B . 1.205(4) ?
O4B C7B . 1.326(4) ?
O4B H4BO . 0.845(10) ?
N1B C5B . 1.336(4) ?
N1B C1B . 1.348(4) ?
C1B C2B . 1.397(4) ?
C1B C6B . 1.525(4) ?
C2B C3B . 1.386(5) ?
C2B C7B . 1.496(5) ?
C3B C4B . 1.367(5) ?
C3B H3B . 0.9300 ?
C4B C5B . 1.398(5) ?
C4B H4B . 0.9300 ?
C5B C8B . 1.497(5) ?
C8B H8BA . 0.9600 ?
C8B H8BB . 0.9600 ?
C8B H8BC . 0.9600 ?
N1C O2C . 1.230(4) ?
N1C O3C . 1.260(4) ?
N1C O1C . 1.261(4) ?
O1M C1M . 1.431(8) ?
O1M H1M . 0.855(10) ?
C1M H1M1 . 0.9600 ?
C1M H1M2 . 0.9600 ?
C1M H1M3 . 0.9600 ?

_cod_database_fobs_code 2240904
