#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:23:29 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/69/2216925.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_2216925
loop_
_publ_author_name
'Lin, Jiao-Min'
'Guan, Yang-Fan'
'Dong, Wen'
_publ_section_title
;
 Bis(2,2'-bipyridine)(5,5'-iminoditetrazolato)cadmium(II)
 2,2'-bipyridine hemisolvate monohydrate
;
_journal_coeditor_code           BQ2057
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m238
_journal_page_last               m238
_journal_paper_doi               10.1107/S1600536807066846
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'2[Cd (C2 H N9) (C10 H8 N2)2], C10 H8 N2, H2 O'
_chemical_formula_moiety         '2(C22 H17 Cd1 N13), C10 H8 N2, 2(H2 O)'
_chemical_formula_sum            'C54 H46 Cd2 N28 O2'
_chemical_formula_weight         1344.00
_chemical_name_systematic
;
Bis(2,2'-bipyridine)(5,5'-iminoditetrazolato)cadmium(II)
2,2'-bipyridine hemisolvate monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.073(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1919(12)
_cell_length_b                   11.2383(9)
_cell_length_c                   17.5759(14)
_cell_measurement_reflns_used    6569
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.994
_cell_measurement_theta_min      27.490
_cell_volume                     2883.5(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2005)'
_computing_publication_material  'SHELXTL (Bruker, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41852
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.296
_refine_ls_extinction_coef       0.00357(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0245
_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)+(0.0274P)²+0.9028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                5669
_reflns_number_total             6569
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bq2057.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C27 H23 Cd N14 O'
_cod_original_formula_weight         672.00
_cod_original_formula_moiety         'C22 H17 Cd1 N13, 0.5(C10 H8 N2), H2 O'
_cod_original_formula_iupac
'[Cd (C2 H N9) (C10 H8 N2)2], 0.5C10 H8 N2, H2 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2216925
_cod_database_fobs_code          2216925
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_refinement_flags
_atom_site_occupancy
Cd Cd1 0.532267(9) 0.270422(13) 0.774688(8) 0.04977(6) Uani d . 1
N N1 0.53723(11) 0.28970(14) 0.64584(10) 0.0532(4) Uani d . 1
N N2 0.56948(13) 0.20365(15) 0.60598(11) 0.0626(4) Uani d . 1
N N6 0.49834(12) 0.46846(15) 0.74874(10) 0.0562(4) Uani d . 1
N N3 0.56653(15) 0.24290(15) 0.53653(11) 0.0669(5) Uani d . 1
N N5 0.48085(12) 0.48791(16) 0.60938(11) 0.0576(4) Uani d . 1
N N9 0.47554(13) 0.64671(15) 0.69592(11) 0.0663(5) Uani d . 1
N N8 0.48433(14) 0.65384(17) 0.77468(12) 0.0714(5) Uani d . 1
N N4 0.53314(12) 0.35578(15) 0.52681(9) 0.0592(4) Uani d . 1
N N7 0.49775(13) 0.54972(17) 0.80637(11) 0.0652(4) Uani d . 1
C C1 0.51621(12) 0.38009(16) 0.59524(10) 0.0479(4) Uani d . 1
C C2 0.48555(12) 0.53204(16) 0.68325(11) 0.0495(4) Uani d . 1
N N10 0.45883(14) 0.27233(15) 0.87647(11) 0.0621(4) Uani d . 1
N N12 0.68118(11) 0.31927(17) 0.85200(11) 0.0624(4) Uani d . 1
N N11 0.39018(11) 0.17392(15) 0.73247(11) 0.0594(4) Uani d . 1
N N13 0.62379(11) 0.09995(15) 0.79609(10) 0.0553(4) Uani d . 1
C C7 0.37105(17) 0.23839(18) 0.85718(15) 0.0639(6) Uani d . 1
C C17 0.74399(14) 0.2331(2) 0.86491(13) 0.0602(5) Uani d . 1
C C12 0.36175(15) 0.1183(2) 0.66307(16) 0.0735(6) Uani d . 1
C C8 0.33420(13) 0.18067(18) 0.77886(14) 0.0606(5) Uani d . 1
C C18 0.71146(13) 0.1114(2) 0.83875(12) 0.0579(5) Uani d . 1
C C16 0.83514(18) 0.2601(3) 0.9003(2) 0.0903(9) Uani d . 1
C C6 0.3187(3) 0.2561(3) 0.9092(2) 0.0921(9) Uani d . 1
C C3 0.4959(2) 0.3204(3) 0.94745(15) 0.0824(7) Uani d . 1
C C11 0.27651(18) 0.0677(3) 0.6357(2) 0.0915(9) Uani d . 1
C C22 0.59252(17) -0.0076(2) 0.77108(16) 0.0703(6) Uani d . 1
C C14 0.79708(19) 0.4612(3) 0.90888(19) 0.0904(8) Uani d . 1
C C15 0.8608(2) 0.3740(3) 0.9222(2) 0.1035(10) Uani d . 1
C C9 0.24676(18) 0.1321(3) 0.7531(2) 0.0864(8) Uani d . 1
C C13 0.70807(17) 0.4305(2) 0.87371(17) 0.0808(7) Uani d . 1
C C19 0.76731(19) 0.0129(3) 0.8578(2) 0.0885(8) Uani d . 1
C C10 0.21877(19) 0.0756(3) 0.6815(2) 0.0998(10) Uani d . 1
C C4 0.4464(4) 0.3369(3) 1.00196(19) 0.1007(11) Uani d . 1
C C21 0.6447(2) -0.1090(2) 0.7879(2) 0.0860(8) Uani d . 1
C C5 0.3577(3) 0.3043(3) 0.9816(2) 0.1103(12) Uani d . 1
C C20 0.7331(2) -0.0975(3) 0.8319(2) 0.1006(10) Uani d . 1
O O1 0.40434(19) 0.8585(2) 0.60636(19) 0.1105(8) Uani d . 1
C C28 0.54281(19) 0.0235(2) 0.02531(14) 0.0757(6) Uani d . 1
C C27 0.5463(2) 0.0710(2) 0.09726(16) 0.0844(7) Uani d . 1
H H21 0.4938 0.0743 0.1147 0.101 Uiso calc R 1
C C26 0.6255(3) 0.1129(3) 0.1425(2) 0.1115(11) Uani d . 1
C C25 0.7028(3) 0.1084(3) 0.1179(2) 0.1102(11) Uani d . 1
N N14 0.6182(2) 0.0168(2) -0.00166(16) 0.1035(8) Uani d . 1
H H1 0.4760(15) 0.533(2) 0.5756(13) 0.062(7) Uiso d . 1
H H9 0.4053(16) 0.116(2) 0.6320(13) 0.072(7) Uiso d . 1
H H6 0.2165(19) 0.139(2) 0.7846(16) 0.087(9) Uiso d . 1
H H7 0.158(2) 0.044(3) 0.6619(17) 0.106(9) Uiso d . 1
H H8 0.260(2) 0.026(3) 0.5852(19) 0.121(11) Uiso d . 1
H H2 0.5629(19) 0.338(3) 0.9605(16) 0.096(9) Uiso d . 1
H H4 0.323(2) 0.316(3) 1.021(2) 0.131(11) Uiso d . 1
H H5 0.259(2) 0.233(3) 0.894(2) 0.105(11) Uiso d . 1
H H3 0.475(2) 0.365(3) 1.0450(19) 0.098(10) Uiso d . 1
H H17 0.5337(17) -0.013(2) 0.7381(14) 0.074(7) Uiso d . 1
H H13 0.874(2) 0.201(3) 0.9080(16) 0.088(9) Uiso d . 1
H H11 0.8101(19) 0.542(3) 0.9196(16) 0.100(9) Uiso d . 1
H H10 0.6577(19) 0.491(2) 0.8614(16) 0.095(9) Uiso d . 1
H H16 0.6172(18) -0.179(3) 0.7664(16) 0.089(8) Uiso d . 1
H H15 0.769(2) -0.165(3) 0.8439(19) 0.121(11) Uiso d . 1
H H12 0.923(2) 0.395(3) 0.9494(19) 0.126(11) Uiso d . 1
H H14 0.828(2) 0.027(3) 0.8895(18) 0.108(10) Uiso d . 1
H H20 0.632(2) 0.143(3) 0.194(2) 0.130(13) Uiso d . 1
H H19 0.764(2) 0.129(3) 0.150(2) 0.125(12) Uiso d . 1
C C24 0.6980(3) 0.0596(4) 0.0460(2) 0.1138(11) Uani d . 1
H H22 0.421(3) 0.801(4) 0.635(2) 0.123(14) Uiso d . 1
H H23 0.398(3) 0.830(4) 0.556(3) 0.163(17) Uiso d . 1
H H18 0.747(2) 0.040(3) 0.0236(19) 0.113(11) Uiso d . 1
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_3
_geom_angle
N1 Cd1 N6 . 77.29(6)
N1 Cd1 N13 . 93.18(6)
N6 Cd1 N13 . 156.31(6)
N1 Cd1 N11 . 90.59(6)
N6 Cd1 N11 . 104.39(6)
N13 Cd1 N11 . 97.26(6)
N1 Cd1 N10 . 154.10(7)
N6 Cd1 N10 . 90.83(6)
N13 Cd1 N10 . 105.73(6)
N11 Cd1 N10 . 69.92(7)
N1 Cd1 N12 . 104.95(6)
N6 Cd1 N12 . 90.89(6)
N13 Cd1 N12 . 70.42(6)
N11 Cd1 N12 . 160.38(7)
N10 Cd1 N12 . 98.09(7)
C1 N1 N2 . 104.62(16)
C1 N1 Cd1 . 131.62(12)
N2 N1 Cd1 . 123.69(12)
N3 N2 N1 . 108.74(16)
C2 N6 N7 . 104.75(16)
C2 N6 Cd1 . 131.75(13)
N7 N6 Cd1 . 123.14(13)
N2 N3 N4 . 110.66(16)
C2 N5 C1 . 124.64(17)
C2 N5 H1 . 117.6(18)
C1 N5 H1 . 113.5(18)
C2 N9 N8 . 104.23(17)
N7 N8 N9 . 110.31(16)
C1 N4 N3 . 103.75(16)
N8 N7 N6 . 108.63(17)
N4 C1 N1 . 112.23(16)
N4 C1 N5 . 121.93(17)
N1 C1 N5 . 125.85(17)
N6 C2 N9 . 112.07(17)
N6 C2 N5 . 125.76(17)
N9 C2 N5 . 122.17(18)
C3 N10 C7 . 119.1(2)
C3 N10 Cd1 . 123.25(19)
C7 N10 Cd1 . 116.97(15)
C17 N12 C13 . 118.86(19)
C17 N12 Cd1 . 117.10(14)
C13 N12 Cd1 . 123.39(16)
C12 N11 C8 . 119.13(19)
C12 N11 Cd1 . 122.94(15)
C8 N11 Cd1 . 117.85(14)
C22 N13 C18 . 118.75(19)
C22 N13 Cd1 . 123.41(14)
C18 N13 Cd1 . 117.78(14)
N10 C7 C6 . 120.5(3)
N10 C7 C8 . 116.96(19)
C6 C7 C8 . 122.6(3)
N12 C17 C16 . 119.7(2)
N12 C17 C18 . 117.10(18)
C16 C17 C18 . 123.2(2)
N11 C12 C11 . 123.4(3)
N11 C12 H9 . 115.5(14)
C11 C12 H9 . 121.1(14)
N11 C8 C9 . 119.5(2)
N11 C8 C7 . 116.84(19)
C9 C8 C7 . 123.7(2)
N13 C18 C19 . 120.5(2)
N13 C18 C17 . 117.10(18)
C19 C18 C17 . 122.3(2)
C15 C16 C17 . 120.4(3)
C15 C16 H13 . 123.0(19)
C17 C16 H13 . 117(2)
C5 C6 C7 . 119.7(4)
C5 C6 H5 . 122(2)
C7 C6 H5 . 119(2)
N10 C3 C4 . 122.2(3)
N10 C3 H2 . 115.7(16)
C4 C3 H2 . 122.0(16)
C10 C11 C12 . 118.0(3)
C10 C11 H8 . 122(2)
C12 C11 H8 . 120(2)
N13 C22 C21 . 123.5(2)
N13 C22 H17 . 117.5(15)
C21 C22 H17 . 118.9(16)
C15 C14 C13 . 117.9(3)
C15 C14 H11 . 124.4(18)
C13 C14 H11 . 117.6(18)
C14 C15 C16 . 119.8(3)
C14 C15 H12 . 118(2)
C16 C15 H12 . 122(2)
C10 C9 C8 . 120.5(3)
C10 C9 H6 . 125(2)
C8 C9 H6 . 114(2)
N12 C13 C14 . 123.4(3)
N12 C13 H10 . 114.6(16)
C14 C13 H10 . 122.0(16)
C20 C19 C18 . 119.6(3)
C20 C19 H14 . 124.2(19)
C18 C19 H14 . 116(2)
C11 C10 C9 . 119.5(3)
C11 C10 H7 . 118.7(18)
C9 C10 H7 . 121.8(18)
C5 C4 C3 . 118.3(3)
C5 C4 H3 . 125(2)
C3 C4 H3 . 116(2)
C20 C21 C22 . 117.7(3)
C20 C21 H16 . 125.4(17)
C22 C21 H16 . 116.9(18)
C4 C5 C6 . 120.2(3)
C4 C5 H4 . 118(2)
C6 C5 H4 . 122(2)
C21 C20 C19 . 119.9(3)
C21 C20 H15 . 119(2)
C19 C20 H15 . 121(2)
H22 O1 H23 . 104(4)
N14 C28 C27 . 121.8(3)
N14 C28 C28 3_655 117.6(3)
C27 C28 C28 3_655 120.5(3)
C26 C27 C28 . 119.3(3)
C26 C27 H21 . 120.3
C28 C27 H21 . 120.3
C27 C26 C25 . 121.0(4)
C27 C26 H20 . 123(2)
C25 C26 H20 . 116(2)
C26 C25 C24 . 118.7(4)
C26 C25 H19 . 126(2)
C24 C25 H19 . 115(2)
C28 N14 C24 . 117.4(3)
N14 C24 C25 . 121.7(4)
N14 C24 H18 . 109(2)
C25 C24 H18 . 129(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 N1 . 2.2970(17)
Cd1 N6 . 2.3015(17)
Cd1 N13 . 2.3357(16)
Cd1 N11 . 2.3451(16)
Cd1 N10 . 2.3559(18)
Cd1 N12 . 2.3587(16)
N1 C1 . 1.329(2)
N1 N2 . 1.362(2)
N2 N3 . 1.287(3)
N6 C2 . 1.322(2)
N6 N7 . 1.366(2)
N3 N4 . 1.359(2)
N5 C2 . 1.373(2)
N5 C1 . 1.376(2)
N5 H1 . 0.77(2)
N9 C2 . 1.324(3)
N9 N8 . 1.356(3)
N8 N7 . 1.288(3)
N4 C1 . 1.326(2)
N10 C3 . 1.333(3)
N10 C7 . 1.337(3)
N12 C17 . 1.334(3)
N12 C13 . 1.338(3)
N11 C12 . 1.332(3)
N11 C8 . 1.333(3)
N13 C22 . 1.328(3)
N13 C18 . 1.341(2)
C7 C6 . 1.382(4)
C7 C8 . 1.484(3)
C17 C16 . 1.386(3)
C17 C18 . 1.483(3)
C12 C11 . 1.373(3)
C12 H9 . 0.97(2)
C8 C9 . 1.391(3)
C18 C19 . 1.378(3)
C16 C15 . 1.362(5)
C16 H13 . 0.88(3)
C6 C5 . 1.358(5)
C6 H5 . 0.91(3)
C3 C4 . 1.384(4)
C3 H2 . 1.00(3)
C11 C10 . 1.348(5)
C11 H8 . 0.97(3)
C22 C21 . 1.373(3)
C22 H17 . 0.92(2)
C14 C15 . 1.352(5)
C14 C13 . 1.366(3)
C14 H11 . 0.93(3)
C15 H12 . 0.96(3)
C9 C10 . 1.367(5)
C9 H6 . 0.82(3)
C13 H10 . 1.00(3)
C19 C20 . 1.373(4)
C19 H14 . 0.95(3)
C10 H7 . 0.96(3)
C4 C5 . 1.346(5)
C4 H3 . 0.82(3)
C21 C20 . 1.357(4)
C21 H16 . 0.92(3)
C5 H4 . 0.98(4)
C20 H15 . 0.92(3)
O1 H22 . 0.82(4)
O1 H23 . 0.92(4)
C28 N14 . 1.357(4)
C28 C27 . 1.361(3)
C28 C28 3_655 1.456(5)
C27 C26 . 1.332(5)
C27 H21 . 0.9300
C26 C25 . 1.360(5)
C26 H20 . 0.94(4)
C25 C24 . 1.361(5)
C25 H19 . 0.97(3)
N14 C24 . 1.357(5)
C24 H18 . 0.96(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N5 H1 N4 3_666 0.77(2) 2.17(2) 2.929(2) 174(2)
O1 H22 N9 . 0.82(4) 2.08(4) 2.893(3) 172(4)
O1 H23 N3 3_666 0.92(4) 2.02(5) 2.901(3) 159(4)
