#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309177.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_4309177
loop_
_publ_author_name
'Md. Badruz Zaman'
'Konstantin Udachin'
'John A. Ripmeester'
'Mark D. Smith'
'Hans-Conrad zur Loye'
_publ_section_title
;
Synthesis and Characterization of Diverse Coordination Polymers. Linear and
Zigzag Chains Involving Their Structural Transformation via Intermolecular
Hydrogen-Bonded, Interpenetrating Ladders Polycatenane, and
Noninterpenetrating Square Grid from Long, Rigid N,N'-Bidentate Ligands:
1,4-Bis[(x-pyridyl)ethynyl]benzene (x= 3 and 4)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5047
_journal_page_last               5059
_journal_paper_doi               10.1021/ic050080d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H28 Co N6 O8'
_chemical_formula_weight         779.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                100.4270(10)
_cell_angle_beta                 97.3240(10)
_cell_angle_gamma                110.9010(10)
_cell_formula_units_Z            1
_cell_length_a                   7.4928(5)
_cell_length_b                   8.9480(5)
_cell_length_c                   14.8543(9)
_cell_measurement_temperature    173(2)
_cell_volume                     894.81(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10592
_diffrn_reflns_theta_full        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            light_pink
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             401
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.513(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         8338
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0434P)²+0.2238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                8040
_reflns_number_total             8338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050080dsi20050119_032607_5.cif
_cod_data_source_block           compound-5_zam98
_cod_original_cell_volume        894.80(9)
_cod_database_code               4309177
loop_
_symmetry_equiv_pos_as_xyz
'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
O1 O 0.39184(5) 0.07793(5) 0.24901(3) 0.02307(11) Uani 1 1 d . A 1
H12W H 0.4511 0.1415 0.3140 0.050 Uiso 1 1 d . B 1
H11W H 0.2759 0.0775 0.2380 0.050 Uiso 1 1 d . C 1
O2 O 0.71987(6) 0.19061(5) 0.04898(3) 0.02292(11) Uani 1 1 d . A 1
H22W H 0.8490 0.2702 0.0515 0.050 Uiso 1 1 d . D 1
H21W H 0.6663 0.1331 -0.0090 0.050 Uiso 1 1 d . E 1
Co1 Co 0.55537(3) 0.13369(2) 0.149208(15) 0.01834(1) Uani 1 1 d . . .
O3 O 0.78359(6) 0.13023(5) 0.25010(3) 0.02783(12) Uani 1 1 d . A .
O4 O 1.03288(7) 0.28140(6) 0.20302(4) 0.04276(16) Uani 1 1 d . A .
O5 O 1.07257(7) 0.16205(7) 0.31490(4) 0.04616(16) Uani 1 1 d . A .
O6 O 0.33026(6) 0.13757(5) 0.04819(3) 0.02604(12) Uani 1 1 d . A .
O7 O 0.07582(8) -0.00874(7) 0.09792(4) 0.04111(17) Uani 1 1 d . A .
O8 O 0.03788(7) 0.10530(7) -0.01562(4) 0.04165(17) Uani 1 1 d . A .
N1 N 0.47824(6) -0.13122(5) 0.09250(3) 0.02030(12) Uani 1 1 d . A .
N2 N 1.55593(8) -0.76327(7) -0.56715(4) 0.03202(16) Uani 1 1 d . . .
N3 N 0.63256(7) 0.39525(6) 0.20459(4) 0.02236(13) Uani 1 1 d . A .
N4 N -0.44241(8) 1.03447(8) 0.86626(4) 0.03298(16) Uani 1 1 d . . .
N5 N 0.96506(7) 0.19173(6) 0.25520(4) 0.02731(14) Uani 1 1 d . . .
N6 N 0.14493(7) 0.07469(7) 0.04332(4) 0.02648(15) Uani 1 1 d . . .
C1 C 0.32267(8) -0.24716(7) 0.11189(4) 0.02595(15) Uani 1 1 d . . .
H1 H 0.2614(11) -0.2084(9) 0.1606(5) 0.0249(19) Uiso 1 1 d . . .
C2 C 0.27795(9) -0.41109(8) 0.08346(5) 0.03042(17) Uani 1 1 d . A .
H2 H 0.1775(13) -0.4676(10) 0.0903(6) 0.039(2) Uiso 1 1 d . . .
C3 C 0.40027(8) -0.46699(7) 0.03075(4) 0.02736(15) Uani 1 1 d . . .
H3 H 0.3847(10) -0.5788(8) 0.0240(5) 0.0206(17) Uiso 1 1 d . . .
C5 C 0.59103(8) -0.18434(7) 0.04402(4) 0.02514(15) Uani 1 1 d . . .
H5 H 0.6907(10) -0.0927(8) 0.0240(5) 0.0212(18) Uiso 1 1 d . . .
C9 C 1.03925(12) -0.35595(9) -0.18138(7) 0.0536(3) Uani 1 1 d . A .
H9 H 1.0402(13) -0.2452(11) -0.1647(6) 0.044(3) Uiso 1 1 d . . .
C10 C 1.15890(12) -0.39484(9) -0.23495(6) 0.0485(2) Uani 1 1 d . . .
H10 H 1.2641(15) -0.2928(12) -0.2547(8) 0.060(3) Uiso 1 1 d . . .
C12 C 1.09388(9) -0.64426(8) -0.18742(4) 0.03059(16) Uani 1 1 d . . .
H12 H 1.1358(13) -0.7352(10) -0.1825(6) 0.040(2) Uiso 1 1 d . . .
C13 C 0.96758(9) -0.60849(7) -0.13368(4) 0.02737(15) Uani 1 1 d . A .
H13 H 0.8818(10) -0.6914(8) -0.1018(5) 0.0189(17) Uiso 1 1 d . . .
C16 C 1.45945(10) -0.70664(8) -0.51108(4) 0.03039(17) Uani 1 1 d . . .
H16 H 1.3386(9) -0.7086(7) -0.5353(4) 0.0097(14) Uiso 1 1 d . . .
C18 C 1.68098(9) -0.69520(8) -0.37466(4) 0.02937(17) Uani 1 1 d . . .
H18 H 1.7139(12) -0.6858(10) -0.3045(6) 0.033(2) Uiso 1 1 d . . .
C19 C 1.77897(9) -0.75454(8) -0.43416(5) 0.03083(17) Uani 1 1 d . . .
H19 H 1.8764(10) -0.7944(8) -0.4107(5) 0.0212(18) Uiso 1 1 d . . .
C20 C 1.70841(10) -0.79105(8) -0.53256(4) 0.03006(17) Uani 1 1 d . . .
H20 H 1.7487(10) -0.8498(8) -0.5762(5) 0.0199(17) Uiso 1 1 d . . .
C21 C 0.78625(9) 0.51089(7) 0.18772(5) 0.02786(17) Uani 1 1 d . . .
H21 H 0.8782(10) 0.4700(8) 0.1615(5) 0.0192(17) Uiso 1 1 d . . .
C22 C 0.82886(10) 0.68176(8) 0.21694(5) 0.03044(18) Uani 1 1 d . A .
H22 H 0.9461(12) 0.7719(10) 0.1981(6) 0.029(2) Uiso 1 1 d . . .
C23 C 0.71719(10) 0.73409(7) 0.26540(5) 0.02766(17) Uani 1 1 d . . .
H23 H 0.7533(10) 0.8456(8) 0.2965(5) 0.0156(17) Uiso 1 1 d . . .
C25 C 0.51796(9) 0.44770(6) 0.25440(4) 0.02303(15) Uani 1 1 d . . .
H25 H 0.3951(10) 0.3729(8) 0.2554(5) 0.0161(17) Uiso 1 1 d . . .
C29 C 0.07746(11) 0.61872(8) 0.48251(6) 0.0430(2) Uani 1 1 d . A .
H29 H 0.1243(12) 0.5318(10) 0.4929(6) 0.031(2) Uiso 1 1 d . . .
C30 C -0.04862(12) 0.65705(9) 0.53684(6) 0.0447(2) Uani 1 1 d . . .
H30 H -0.0849(12) 0.6027(10) 0.5863(6) 0.033(2) Uiso 1 1 d . . .
C32 C 0.01951(10) 0.91205(8) 0.48600(5) 0.03148(18) Uani 1 1 d . . .
H32 H 0.0211(11) 1.0258(9) 0.4959(5) 0.0241(19) Uiso 1 1 d . . .
C33 C 0.13980(10) 0.86997(9) 0.43224(5) 0.03195(19) Uani 1 1 d . A .
H33 H 0.1722(13) 0.9285(11) 0.3850(7) 0.041(2) Uiso 1 1 d . . .
C37 C -0.57162(9) 0.96629(8) 0.67408(4) 0.02670(16) Uani 1 1 d . . .
H37 H -0.6263(12) 0.9343(10) 0.6124(6) 0.030(2) Uiso 1 1 d . . .
C38 C -0.67182(9) 1.02447(8) 0.73568(5) 0.02995(17) Uani 1 1 d . . .
H38 H -0.8057(11) 1.0167(9) 0.7130(5) 0.0244(19) Uiso 1 1 d . . .
C39 C -0.60480(9) 1.05508(8) 0.82837(5) 0.03106(18) Uani 1 1 d . . .
H39 H -0.6906(11) 1.0796(9) 0.8731(5) 0.0250(19) Uiso 1 1 d . . .
C40 C -0.35055(9) 0.97311(9) 0.80441(5) 0.03260(18) Uani 1 1 d . . .
H40 H -0.2555(13) 0.9179(11) 0.8384(6) 0.041(2) Uiso 1 1 d . . .
C4 C 0.55393(8) -0.35038(7) 0.01204(4) 0.02568(14) Uani 1 1 d . A .
C6 C 0.69072(9) -0.39303(8) -0.03929(5) 0.03120(17) Uani 1 1 d . . .
C7 C 0.80392(10) -0.42541(8) -0.08109(5) 0.03317(18) Uani 1 1 d . A .
C8 C 0.93911(9) -0.45796(7) -0.13344(5) 0.02976(16) Uani 1 1 d . . .
C11 C 1.18518(9) -0.54215(7) -0.23982(5) 0.02966(16) Uani 1 1 d . . .
C14 C 1.30885(10) -0.58155(8) -0.29850(4) 0.03229(18) Uani 1 1 d . . .
C15 C 1.40081(10) -0.61947(8) -0.35210(4) 0.03088(17) Uani 1 1 d . . .
C17 C 1.51759(8) -0.67333(7) -0.41170(4) 0.02587(15) Uani 1 1 d . . .
C24 C 0.55123(9) 0.61568(7) 0.28719(4) 0.02388(16) Uani 1 1 d . A .
C26 C 0.42334(10) 0.65933(7) 0.33687(5) 0.02915(18) Uani 1 1 d . . .
C27 C 0.30701(10) 0.68984(8) 0.37737(5) 0.03172(18) Uani 1 1 d . A .
C28 C 0.17377(10) 0.73103(8) 0.42913(5) 0.02924(18) Uani 1 1 d . . .
C31 C -0.07864(9) 0.80209(8) 0.53915(4) 0.02825(17) Uani 1 1 d . . .
C34 C -0.19641(9) 0.84809(8) 0.59984(5) 0.02974(18) Uani 1 1 d . . .
C35 C -0.29507(9) 0.88510(9) 0.64978(5) 0.02983(18) Uani 1 1 d . . .
C36 C -0.40500(9) 0.93823(8) 0.71009(4) 0.02604(16) Uani 1 1 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'
Co Co 0.3494 0.9721 '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 Co1 O2 179.80(2) . . ?
O1 Co1 O6 96.83(2) . . ?
O2 Co1 O6 83.12(2) . . ?
O1 Co1 O3 83.65(2) . . ?
O2 Co1 O3 96.40(2) . . ?
O6 Co1 O3 179.52(2) . . ?
O1 Co1 N3 90.84(2) . . ?
O2 Co1 N3 88.97(2) . . ?
O6 Co1 N3 87.63(2) . . ?
O3 Co1 N3 92.374(19) . . ?
O1 Co1 N1 89.486(19) . . ?
O2 Co1 N1 90.71(2) . . ?
O6 Co1 N1 92.364(19) . . ?
O3 Co1 N1 87.626(19) . . ?
N3 Co1 N1 179.68(3) . . ?
N5 O3 Co1 128.54(4) . . ?
N6 O6 Co1 127.87(4) . . ?
C5 N1 C1 117.36(5) . . ?
C5 N1 Co1 121.18(4) . . ?
C1 N1 Co1 121.26(4) . . ?
C20 N2 C16 120.45(6) . . ?
C21 N3 C25 116.98(5) . . ?
C21 N3 Co1 122.57(5) . . ?
C25 N3 Co1 120.37(4) . . ?
C39 N4 C40 116.27(6) . . ?
O4 N5 O5 121.84(5) . . ?
O4 N5 O3 120.02(6) . . ?
O5 N5 O3 118.12(6) . . ?
O7 N6 O8 121.07(6) . . ?
O7 N6 O6 120.93(6) . . ?
O8 N6 O6 117.94(6) . . ?
C2 C1 N1 123.04(6) . . ?
C1 C2 C3 119.09(6) . . ?
C4 C3 C2 117.11(6) . . ?
N1 C5 C4 122.92(5) . . ?
C8 C9 C10 122.02(8) . . ?
C9 C10 C11 120.82(8) . . ?
C11 C12 C13 121.57(7) . . ?
C12 C13 C8 118.01(6) . . ?
N2 C16 C17 121.13(7) . . ?
C19 C18 C17 118.92(6) . . ?
C18 C19 C20 119.03(7) . . ?
N2 C20 C19 121.37(7) . . ?
N3 C21 C22 123.06(7) . . ?
C23 C22 C21 120.33(6) . . ?
C22 C23 C24 119.27(6) . . ?
N3 C25 C24 123.62(5) . . ?
C30 C29 C28 119.30(7) . . ?
C31 C30 C29 120.23(8) . . ?
C33 C32 C31 119.05(7) . . ?
C28 C33 C32 123.05(7) . . ?
C38 C37 C36 119.67(6) . . ?
C39 C38 C37 118.70(7) . . ?
C38 C39 N4 123.74(7) . . ?
C36 C40 N4 124.91(7) . . ?
C3 C4 C5 120.47(6) . . ?
C3 C4 C6 121.77(6) . . ?
C5 C4 C6 117.73(5) . . ?
C7 C6 C4 179.02(7) . . ?
C6 C7 C8 177.16(8) . . ?
C9 C8 C7 123.44(7) . . ?
C9 C8 C13 118.95(7) . . ?
C7 C8 C13 117.61(6) . . ?
C12 C11 C10 118.48(7) . . ?
C12 C11 C14 121.93(7) . . ?
C10 C11 C14 119.59(7) . . ?
C15 C14 C11 175.58(6) . . ?
C14 C15 C17 174.99(8) . . ?
C18 C17 C16 118.99(6) . . ?
C18 C17 C15 121.48(6) . . ?
C16 C17 C15 119.52(6) . . ?
C26 C24 C25 119.98(6) . . ?
C26 C24 C23 123.30(6) . . ?
C25 C24 C23 116.71(6) . . ?
C27 C26 C24 176.98(6) . . ?
C26 C27 C28 177.65(7) . . ?
C33 C28 C29 118.93(7) . . ?
C33 C28 C27 123.67(7) . . ?
C29 C28 C27 117.37(7) . . ?
C30 C31 C32 119.43(7) . . ?
C30 C31 C34 120.55(7) . . ?
C32 C31 C34 119.86(7) . . ?
C35 C34 C31 179.52(7) . . ?
C34 C35 C36 176.85(7) . . ?
C40 C36 C37 116.65(7) . . ?
C40 C36 C35 122.00(7) . . ?
C37 C36 C35 121.26(6) . . ?
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
O1 Co1 2.0599(5) . ?
O2 Co1 2.0711(5) . ?
Co1 O6 2.1244(5) . ?
Co1 O3 2.1383(5) . ?
Co1 N3 2.1690(6) . ?
Co1 N1 2.1996(5) . ?
O3 N5 1.2579(7) . ?
O4 N5 1.2400(8) . ?
O5 N5 1.2496(8) . ?
O6 N6 1.2855(7) . ?
O7 N6 1.2384(8) . ?
O8 N6 1.2447(9) . ?
N1 C5 1.3329(8) . ?
N1 C1 1.3597(7) . ?
N2 C20 1.3155(10) . ?
N2 C16 1.3172(10) . ?
N3 C21 1.3330(8) . ?
N3 C25 1.3523(9) . ?
N4 C39 1.3617(10) . ?
N4 C40 1.3665(10) . ?
C1 C2 1.3533(9) . ?
C2 C3 1.4392(10) . ?
C3 C4 1.3495(8) . ?
C5 C4 1.3880(9) . ?
C9 C8 1.3365(12) . ?
C9 C10 1.3647(14) . ?
C10 C11 1.3913(12) . ?
C12 C11 1.3622(10) . ?
C12 C13 1.3969(10) . ?
C13 C8 1.4364(10) . ?
C16 C17 1.4290(8) . ?
C18 C19 1.3697(10) . ?
C18 C17 1.3703(10) . ?
C19 C20 1.4246(9) . ?
C21 C22 1.4157(9) . ?
C22 C23 1.3224(11) . ?
C23 C24 1.4355(9) . ?
C25 C24 1.4126(8) . ?
C29 C30 1.4095(13) . ?
C29 C28 1.4409(11) . ?
C30 C31 1.3894(12) . ?
C32 C33 1.3816(11) . ?
C32 C31 1.4300(10) . ?
C33 C28 1.3493(12) . ?
C37 C38 1.3977(10) . ?
C37 C36 1.4177(11) . ?
C38 C39 1.3460(10) . ?
C40 C36 1.3534(10) . ?
C4 C6 1.4665(10) . ?
C6 C7 1.1972(11) . ?
C7 C8 1.4301(11) . ?
C11 C14 1.4389(10) . ?
C14 C15 1.1970(11) . ?
C15 C17 1.4580(10) . ?
C24 C26 1.3994(11) . ?
C26 C27 1.2001(11) . ?
C27 C28 1.4420(11) . ?
C31 C34 1.4452(11) . ?
C34 C35 1.1967(11) . ?
C35 C36 1.4215(10) . ?
