#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/37/4113781.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_4113781
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         'C20.80 H19.60 Cd N4 O7'
_chemical_formula_sum            'C20.8 H19.6 Cd N4 O7'
_chemical_formula_weight         550.00
_chemical_name_common            Bipy*Cd(NO3)2*i-PrOH
_chemical_name_systematic
; 
 1-(4-Pyridyl)-4(2-pyridylethynyl)benzene cadmium(II) 
bisnitrate complex isopropanol solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens
'OH-proton found from difference electron map, others placed geometrically'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier methods'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.657(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2770(8)
_cell_length_b                   13.2606(8)
_cell_length_c                   14.3240(8)
_cell_measurement_reflns_used    5832
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.28
_cell_volume                     2292.0(2)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'Bruker SMART1000 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  0.027
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13556
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999b)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.72
_refine_diff_density_rms         0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment
'OH-proton freely refined, riding model for others'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.06P)²+0.74P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                4009
_reflns_number_total             5247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029048ysi20021022_034217_7.cif
_cod_data_source_block           (7)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct method' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2292.0(4)
_cod_original_formula_sum        'C20.80 H19.60 Cd N4 O7'
_cod_database_code               4113781
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.189488(19) 0.586259(17) 0.969007(18) 0.02568(9) Uani 1 1 d DU . .
N1 N 0.7367(2) 1.2568(2) 1.0082(2) 0.0266(6) Uani 1 1 d U . .
N10A N -0.0329(2) 0.5859(2) 0.8136(2) 0.0290(6) Uani 1 1 d U . .
N20A N 0.3045(3) 0.4417(2) 1.1196(2) 0.0363(7) Uani 1 1 d U . .
N20 N 0.2404(2) 0.4854(2) 0.8618(2) 0.0283(6) Uani 1 1 d U A .
O1S O 0.1289(3) 0.6324(2) 1.0952(2) 0.0358(7) Uani 0.80 1 d PDU A 1
O11 O 0.0079(2) 0.51691(19) 0.8804(2) 0.0348(6) Uani 1 1 d DU A .
O12 O -0.1278(2) 0.5802(2) 0.7478(2) 0.0440(7) Uani 1 1 d U A .
O13 O 0.0285(2) 0.6600(2) 0.8193(2) 0.0432(7) Uani 1 1 d U A .
O21 O 0.3508(2) 0.5227(2) 1.1114(2) 0.0394(6) Uani 1 1 d U A .
O22 O 0.3548(3) 0.3794(2) 1.1861(2) 0.0469(7) Uani 1 1 d U A .
O23 O 0.2058(2) 0.4273(2) 1.0567(2) 0.0461(7) Uani 1 1 d U A .
C1S C 0.0637(5) 0.7311(5) 1.1110(5) 0.0680(17) Uani 0.80 1 d PDU A 1
H1SA H 0.0335 0.7115 1.1617 0.082 Uiso 0.80 1 calc PR A 1
C2 C 0.7813(3) 1.1800(3) 1.0733(3) 0.0285(7) Uani 1 1 d U B 1
H2A H 0.8455 1.1926 1.1347 0.034 Uiso 1 1 calc R B 1
C2S C 0.1383(7) 0.8140(5) 1.1554(5) 0.071(2) Uani 0.80 1 d PDU A 1
H2SA H 0.0969 0.8716 1.1644 0.107 Uiso 0.80 1 calc PR A 1
H2SB H 0.1733 0.8331 1.1098 0.107 Uiso 0.80 1 calc PR A 1
H2SC H 0.1955 0.7937 1.2223 0.107 Uiso 0.80 1 calc PR A 1
C3 C 0.7388(3) 1.0841(3) 1.0553(3) 0.0305(7) Uani 1 1 d U B 1
H3A H 0.7729 1.0326 1.1045 0.037 Uiso 1 1 calc R B 1
C3S C -0.0310(4) 0.7601(4) 1.0168(4) 0.0519(14) Uani 0.80 1 d PDU A 1
H3SA H -0.0676 0.8188 1.0304 0.078 Uiso 0.80 1 calc PR A 1
H3SB H -0.0835 0.7038 0.9932 0.078 Uiso 0.80 1 calc PR A 1
H3SC H -0.0054 0.7769 0.9637 0.078 Uiso 0.80 1 calc PR A 1
C4 C 0.6456(3) 1.0617(2) 0.9654(3) 0.0272(7) Uani 1 1 d U . .
C5 C 0.6014(3) 1.1413(3) 0.8973(3) 0.0360(9) Uani 1 1 d U B .
H5A H 0.5388 1.1303 0.8342 0.043 Uiso 1 1 calc R . .
C6 C 0.6480(3) 1.2362(3) 0.9210(3) 0.0355(8) Uani 1 1 d U B .
H6A H 0.6157 1.2893 0.8733 0.043 Uiso 1 1 calc R . .
C7 C 0.5950(3) 0.9596(3) 0.9444(3) 0.0286(7) Uani 1 1 d U B .
C8 C 0.6501(4) 0.8756(3) 1.0007(3) 0.0445(10) Uani 1 1 d U . .
H8A H 0.7232 0.8828 1.0527 0.053 Uiso 1 1 calc R B .
C9 C 0.5999(4) 0.7813(3) 0.9821(3) 0.0445(10) Uani 1 1 d U B .
H9A H 0.6390 0.7249 1.0212 0.053 Uiso 1 1 calc R . .
C10 C 0.4931(3) 0.7689(3) 0.9069(3) 0.0315(8) Uani 1 1 d U . .
C11 C 0.4384(3) 0.8523(3) 0.8494(3) 0.0323(8) Uani 1 1 d U B .
H11A H 0.3659 0.8447 0.7965 0.039 Uiso 1 1 calc R . .
C12 C 0.4883(3) 0.9460(3) 0.8682(3) 0.0310(8) Uani 1 1 d U . .
H12A H 0.4492 1.0022 0.8286 0.037 Uiso 1 1 calc R B .
C13 C 0.4385(3) 0.6726(3) 0.8900(3) 0.0320(8) Uani 1 1 d U B .
C14 C 0.3889(3) 0.5951(2) 0.8749(3) 0.0304(7) Uani 1 1 d U . .
C15 C 0.3321(3) 0.5006(2) 0.8446(3) 0.0279(7) Uani 1 1 d U A .
C16 C 0.3693(4) 0.4291(3) 0.7945(3) 0.0392(9) Uani 1 1 d U . .
H16A H 0.4351 0.4408 0.7851 0.047 Uiso 1 1 calc R B .
C17 C 0.3097(4) 0.3418(3) 0.7588(3) 0.0456(10) Uani 1 1 d U B .
H17A H 0.3330 0.2929 0.7236 0.055 Uiso 1 1 calc R . .
C18 C 0.2155(4) 0.3266(3) 0.7752(3) 0.0425(9) Uani 1 1 d U . .
H18A H 0.1727 0.2670 0.7509 0.051 Uiso 1 1 calc R B .
C19 C 0.1840(3) 0.3989(3) 0.8274(3) 0.0355(8) Uani 1 1 d U A .
H19A H 0.1199 0.3869 0.8394 0.043 Uiso 1 1 calc R . .
H1S H 0.105(3) 0.5853(13) 1.110(2) 0.001(8) Uiso 0.80 1 d PD . .
C2S' C -0.087(2) 0.9181(17) 0.9752(17) 0.059(6) Uiso 0.20 1 d PDU C 2
O1S' O 0.0892(19) 0.900(2) 1.106(3) 0.141(12) Uiso 0.20 1 d PDU C 2
C1S' C -0.0311(15) 0.8474(14) 1.0565(14) 0.039(4) Uiso 0.20 1 d PDU C 2
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 113.23(10) 3_677 . y
N1 Cd1 O1S 85.18(10) 3_677 . y
N20 Cd1 O1S 160.22(11) . . y
N1 Cd1 O11 135.20(9) 3_677 . y
N20 Cd1 O11 86.27(10) . . y
O1S Cd1 O11 85.13(10) . . y
N1 Cd1 O21 91.19(9) 3_677 . y
N20 Cd1 O21 87.56(10) . . y
O1S Cd1 O21 84.77(11) . . y
O11 Cd1 O21 131.16(9) . . y
N1 Cd1 O23 141.89(10) 3_677 . y
N20 Cd1 O23 81.62(10) . . y
O1S Cd1 O23 79.18(11) . . y
O11 Cd1 O23 78.02(9) . . y
O21 Cd1 O23 53.16(9) . . y
N1 Cd1 O13 85.89(9) 3_677 . y
N20 Cd1 O13 92.19(10) . . y
O1S Cd1 O13 96.49(11) . . y
O11 Cd1 O13 52.07(8) . . y
O21 Cd1 O13 176.71(9) . . y
O23 Cd1 O13 130.05(9) . . y
C6 N1 C2 117.0(3) . . ?
C6 N1 Cd1 118.8(2) . 3_677 ?
C2 N1 Cd1 124.0(2) . 3_677 ?
O12 N10A O13 122.2(3) . . ?
O12 N10A O11 120.9(3) . . ?
O13 N10A O11 116.9(3) . . ?
O22 N20A O23 121.4(3) . . ?
O22 N20A O21 121.0(3) . . ?
O23 N20A O21 117.6(3) . . ?
C19 N20 C15 117.7(3) . . ?
C19 N20 Cd1 117.3(3) . . ?
C15 N20 Cd1 124.2(2) . . ?
C1S O1S Cd1 133.3(3) . . ?
N10A O11 Cd1 98.12(19) . . ?
N10A O13 Cd1 92.85(19) . . ?
N20A O21 Cd1 94.6(2) . . ?
N20A O23 Cd1 94.6(2) . . ?
C2S C1S C3S 112.1(6) . . ?
C2S C1S O1S 111.5(5) . . ?
C3S C1S O1S 112.6(5) . . ?
N1 C2 C3 123.1(3) . . ?
C2 C3 C4 120.5(3) . . ?
C5 C4 C3 115.9(3) . . ?
C5 C4 C7 121.9(3) . . ?
C3 C4 C7 122.2(3) . . ?
C6 C5 C4 120.4(3) . . ?
N1 C6 C5 123.0(3) . . ?
C8 C7 C12 117.9(3) . . ?
C8 C7 C4 121.9(3) . . ?
C12 C7 C4 120.2(3) . . ?
C9 C8 C7 121.0(4) . . ?
C10 C9 C8 120.6(4) . . ?
C9 C10 C11 118.6(3) . . ?
C9 C10 C13 121.1(3) . . ?
C11 C10 C13 120.3(3) . . ?
C12 C11 C10 120.7(3) . . ?
C11 C12 C7 121.2(3) . . ?
C14 C13 C10 177.1(4) . . ?
C13 C14 C15 172.4(4) . . ?
N20 C15 C16 121.9(3) . . ?
N20 C15 C14 118.4(3) . . ?
C16 C15 C14 119.6(3) . . ?
C17 C16 C15 119.3(4) . . ?
C16 C17 C18 118.8(4) . . ?
C17 C18 C19 119.3(4) . . ?
N20 C19 C18 122.8(4) . . ?
C2S' C1S' O1S' 99(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
Cd1 N1 2.265(3) 3_677 y
Cd1 N20 2.339(3) . y
Cd1 O1S 2.346(3) . y
Cd1 O11 2.391(2) . y
Cd1 O21 2.411(3) . y
Cd1 O23 2.417(3) . y
Cd1 O13 2.510(3) . y
N1 C6 1.339(5) . ?
N1 C2 1.340(4) . ?
N1 Cd1 2.265(3) 3_677 ?
N10A O12 1.221(4) . ?
N10A O13 1.256(4) . ?
N10A O11 1.271(4) . ?
N20A O22 1.226(4) . ?
N20A O23 1.257(4) . ?
N20A O21 1.268(4) . ?
N20 C19 1.346(4) . ?
N20 C15 1.355(4) . ?
O1S C1S 1.637(8) . ?
C1S C2S 1.438(7) . ?
C1S C3S 1.460(7) . ?
C2 C3 1.372(5) . ?
C3 C4 1.396(5) . ?
C4 C5 1.390(5) . ?
C4 C7 1.485(5) . ?
C5 C6 1.381(5) . ?
C7 C8 1.390(5) . ?
C7 C12 1.393(5) . ?
C8 C9 1.390(5) . ?
C9 C10 1.387(6) . ?
C10 C11 1.389(5) . ?
C10 C13 1.438(5) . ?
C11 C12 1.380(5) . ?
C13 C14 1.191(5) . ?
C14 C15 1.433(5) . ?
C15 C16 1.398(5) . ?
C16 C17 1.375(5) . ?
C17 C18 1.381(6) . ?
C18 C19 1.383(5) . ?
C2S' C1S' 1.437(10) . ?
O1S' C1S' 1.608(10) . ?
