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#$Date: 2016-03-22 11:37:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178908 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/37/4113779.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_4113779
loop_
_publ_author_name
'Andrei N. Khlobystov'
'Matthew T. Brett'
'Alexander J. Blake'
'Neil R. Champness'
'Peter M. W. Gill'
'Darragh P. O'Neill'
'Simon J. Teat'
'Claire Wilson'
'Martin Schröder'
_publ_contact_author_address
;
  School of Chemistry
  The University of Nottingham
  University Park
  Nottingham  NG7 2RD
  England
;
_publ_contact_author_email       A.J.Blake@nottingham.ac.uk
_publ_contact_author_fax         '0115 951 3563'
_publ_contact_author_name        'Dr A.J. Blake'
_publ_contact_author_phone       '0115 951 3488'
_publ_section_title
;
 Stereoselective Association of Binuclear Metallacycles in Coordination
 Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6753
_journal_page_last               6761
_journal_paper_doi               10.1021/ja029048y
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C18 H12 N2 Cd 2+, 2(N O3 -), C2 H3 N'
_chemical_formula_sum            'C20 H15 Cd N5 O6'
_chemical_formula_weight         533.77
_chemical_name_common            Cd(NO3)2*Pyyne
_chemical_name_systematic
; 
 1(4-Pyridyl)-4(2-pyridylethynyl)benzene Cadmium bisnitrate complex 
 acetonitrile solvate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens
'Me-group from delta-F synthesis, others placed geometrically'
_atom_sites_solution_primary     'Patterson method'
_atom_sites_solution_secondary   'difference Fourier method'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.583(5)
_cell_length_b                   8.1430(16)
_cell_length_c                   21.270(4)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      3.15
_cell_volume                     4098.4(17)
_computing_cell_refinement       'SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17871
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  10
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       column
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.32
_refine_diff_density_min         -0.40
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment
'rigid rotator for Me-group, riding model for others'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.051P)²+4.524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                4030
_reflns_number_total             4928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029048ysi20021022_034217_5.cif
_cod_data_source_block           (5)
_cod_original_cell_volume        4098.3(14)
_cod_database_code               4113779
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'
'-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
Cd1 Cd 0.823851(9) 0.86324(3) 1.220787(10) 0.02257(8) Uani 1 1 d .
N1 N 1.10238(10) 0.1612(3) 1.66990(13) 0.0233(5) Uani 1 1 d .
N1S N 0.85588(14) 0.5916(4) 1.53126(17) 0.0367(7) Uani 1 1 d D
N10A N 0.89884(11) 0.9461(4) 1.16159(14) 0.0311(6) Uani 1 1 d .
N20A N 0.75686(10) 1.1357(3) 1.22140(13) 0.0242(5) Uani 1 1 d .
N20 N 0.76736(10) 0.6992(3) 1.12889(13) 0.0259(5) Uani 1 1 d .
O11 O 0.89534(11) 0.7962(3) 1.17342(12) 0.0397(6) Uani 1 1 d .
O12 O 0.92843(12) 0.9941(4) 1.13484(16) 0.0546(8) Uani 1 1 d .
O13 O 0.86930(10) 1.0464(3) 1.17634(13) 0.0384(6) Uani 1 1 d .
O21 O 0.79649(9) 1.1000(3) 1.27969(12) 0.0321(5) Uani 1 1 d .
O22 O 0.72293(9) 1.2475(3) 1.21396(12) 0.0328(5) Uani 1 1 d .
O23 O 0.75114(9) 1.0558(3) 1.16773(11) 0.0331(5) Uani 1 1 d .
C1S C 0.8895(2) 0.5839(6) 1.5902(3) 0.0753(18) Uani 1 1 d D
C2 C 1.05130(12) 0.2144(4) 1.65890(15) 0.0260(6) Uani 1 1 d .
H2A H 1.0449 0.2314 1.6979 0.031 Uiso 1 1 calc R
C2S C 0.9414(2) 0.5803(5) 1.6628(2) 0.0656(14) Uani 1 1 d D
H2SA H 0.9749 0.5963 1.6572 0.098 Uiso 1 1 calc R
H2SB H 0.9434 0.4761 1.6848 0.098 Uiso 1 1 calc R
H2SS H 0.9384 0.6664 1.6917 0.098 Uiso 1 1 calc R
C3 C 1.00776(13) 0.2452(4) 1.59252(15) 0.0272(6) Uani 1 1 d .
H3A H 0.9728 0.2801 1.5875 0.033 Uiso 1 1 calc R
C4 C 1.01632(12) 0.2238(4) 1.53291(15) 0.0228(6) Uani 1 1 d .
C5 C 1.06867(12) 0.1620(4) 1.54467(15) 0.0250(6) Uani 1 1 d .
H5A H 1.0761 0.1409 1.5067 0.030 Uiso 1 1 calc R
C6 C 1.10976(13) 0.1319(4) 1.61293(16) 0.0259(6) Uani 1 1 d .
H6A H 1.1442 0.0891 1.6194 0.031 Uiso 1 1 calc R
C7 C 0.97222(11) 0.2696(3) 1.46127(14) 0.0215(6) Uani 1 1 d .
C8 C 0.97279(13) 0.2069(4) 1.40040(15) 0.0272(6) Uani 1 1 d .
H8A H 1.0004 0.1311 1.4048 0.033 Uiso 1 1 calc R
C9 C 0.93319(13) 0.2554(4) 1.33390(15) 0.0275(6) Uani 1 1 d .
H9A H 0.9342 0.2121 1.2941 0.033 Uiso 1 1 calc R
C10 C 0.89147(12) 0.3698(3) 1.32641(15) 0.0242(6) Uani 1 1 d .
C11 C 0.88999(13) 0.4319(4) 1.38671(16) 0.0294(7) Uani 1 1 d .
H11A H 0.8623 0.5072 1.3824 0.035 Uiso 1 1 calc R
C12 C 0.92974(13) 0.3811(4) 1.45280(16) 0.0275(7) Uani 1 1 d .
H12A H 0.9281 0.4223 1.4926 0.033 Uiso 1 1 calc R
C13 C 0.85101(13) 0.4260(4) 1.25771(16) 0.0258(6) Uani 1 1 d .
C14 C 0.81722(13) 0.4741(4) 1.20104(16) 0.0263(6) Uani 1 1 d .
C15 C 0.77421(12) 0.5350(4) 1.13458(15) 0.0257(6) Uani 1 1 d .
C16 C 0.74081(14) 0.4289(4) 1.08005(16) 0.0316(7) Uani 1 1 d .
H16A H 0.7469 0.3162 1.0848 0.038 Uiso 1 1 calc R
C17 C 0.69832(14) 0.4942(4) 1.01864(17) 0.0342(7) Uani 1 1 d .
H17A H 0.6755 0.4258 0.9815 0.041 Uiso 1 1 calc R
C18 C 0.69035(15) 0.6619(4) 1.01331(17) 0.0343(8) Uani 1 1 d .
H18A H 0.6617 0.7083 0.9729 0.041 Uiso 1 1 calc R
C19 C 0.72558(14) 0.7597(4) 1.06909(16) 0.0312(7) Uani 1 1 d .
H19A H 0.7202 0.8728 1.0651 0.037 Uiso 1 1 calc R
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N20 138.85(9) 5_768 . y
N1 Cd1 O23 133.78(9) 5_768 . y
N20 Cd1 O23 84.40(9) . . y
N1 Cd1 O13 96.00(9) 5_768 . y
N20 Cd1 O13 106.47(9) . . y
O23 Cd1 O13 81.09(9) . . y
N1 Cd1 O22 79.00(8) 5_768 4_647 y
N20 Cd1 O22 87.36(8) . 4_647 y
O23 Cd1 O22 90.57(8) . 4_647 y
O13 Cd1 O22 162.92(8) . 4_647 y
N1 Cd1 O21 82.59(8) 5_768 . y
N20 Cd1 O21 129.35(8) . . y
O23 Cd1 O21 51.66(7) . . y
O13 Cd1 O21 91.78(8) . . y
O22 Cd1 O21 71.46(7) 4_647 . y
N1 Cd1 O11 86.28(9) 5_768 . y
N20 Cd1 O11 81.71(9) . . y
O23 Cd1 O11 123.11(8) . . y
O13 Cd1 O11 51.54(8) . . y
O22 Cd1 O11 142.95(8) 4_647 . y
O21 Cd1 O11 140.21(8) . . y
C6 N1 C2 117.1(3) . . ?
C6 N1 Cd1 120.0(2) . 5_768 ?
C2 N1 Cd1 122.8(2) . 5_768 ?
O12 N10A O11 121.6(3) . . ?
O12 N10A O13 120.6(3) . . ?
O11 N10A O13 117.7(3) . . ?
O22 N20A O21 122.4(3) . . ?
O22 N20A O23 118.9(3) . . ?
O21 N20A O23 118.7(2) . . ?
C19 N20 C15 117.9(3) . . ?
C19 N20 Cd1 122.3(2) . . ?
C15 N20 Cd1 119.72(19) . . ?
N10A O11 Cd1 90.44(18) . . ?
N10A O13 Cd1 100.29(19) . . ?
N20A O21 Cd1 89.37(17) . . ?
N20A O22 Cd1 137.90(19) . 4_657 ?
N20A O23 Cd1 100.19(17) . . ?
N1S C1S C2S 169.7(5) . . ?
N1 C2 C3 123.2(3) . . ?
C2 C3 C4 119.9(3) . . ?
C5 C4 C3 116.4(3) . . ?
C5 C4 C7 122.2(3) . . ?
C3 C4 C7 121.4(3) . . ?
C6 C5 C4 119.9(3) . . ?
N1 C6 C5 123.3(3) . . ?
C12 C7 C8 117.9(3) . . ?
C12 C7 C4 120.7(3) . . ?
C8 C7 C4 121.4(3) . . ?
C9 C8 C7 121.3(3) . . ?
C8 C9 C10 120.1(3) . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 C13 119.8(3) . . ?
C9 C10 C13 120.9(3) . . ?
C12 C11 C10 119.9(3) . . ?
C11 C12 C7 121.7(3) . . ?
C14 C13 C10 179.2(4) . . ?
C13 C14 C15 176.4(3) . . ?
N20 C15 C16 122.1(3) . . ?
N20 C15 C14 116.4(3) . . ?
C16 C15 C14 121.5(3) . . ?
C17 C16 C15 118.9(3) . . ?
C18 C17 C16 119.1(3) . . ?
C17 C18 C19 118.8(3) . . ?
N20 C19 C18 123.1(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
Cd1 N1 2.266(3) 5_768 y
Cd1 N20 2.277(3) . y
Cd1 O23 2.341(2) . y
Cd1 O13 2.371(2) . y
Cd1 O22 2.436(2) 4_647 y
Cd1 O21 2.578(2) . y
Cd1 O11 2.583(3) . y
N1 C6 1.334(4) . ?
N1 C2 1.340(4) . ?
N1 Cd1 2.266(3) 5_768 ?
N1S C1S 1.164(6) . ?
N10A O12 1.226(4) . ?
N10A O11 1.258(4) . ?
N10A O13 1.268(4) . ?
N20A O22 1.240(3) . ?
N20A O21 1.241(3) . ?
N20A O23 1.262(3) . ?
N20 C19 1.344(4) . ?
N20 C15 1.347(4) . ?
O22 Cd1 2.436(2) 4_657 ?
C1S C2S 1.531(6) . ?
C2 C3 1.381(4) . ?
C3 C4 1.397(4) . ?
C4 C5 1.391(4) . ?
C4 C7 1.486(4) . ?
C5 C6 1.384(4) . ?
C7 C12 1.395(4) . ?
C7 C8 1.398(4) . ?
C8 C9 1.381(4) . ?
C9 C10 1.401(4) . ?
C10 C11 1.396(4) . ?
C10 C13 1.438(4) . ?
C11 C12 1.382(4) . ?
C13 C14 1.194(4) . ?
C14 C15 1.442(4) . ?
C15 C16 1.393(4) . ?
C16 C17 1.386(4) . ?
C17 C18 1.379(5) . ?
C18 C19 1.381(5) . ?
