#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309175.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_4309175
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 H24 Cu N6 O6'
_chemical_formula_weight         748.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                107.9910(10)
_cell_angle_beta                 97.1090(10)
_cell_angle_gamma                115.5420(10)
_cell_formula_units_Z            1
_cell_length_a                   8.7280(5)
_cell_length_b                   10.0176(6)
_cell_length_c                   11.8926(7)
_cell_measurement_temperature    173(2)
_cell_volume                     851.39(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10131
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             383
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0433P)²+0.1897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                3711
_reflns_number_total             4369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050080dsi20050119_032607_3.cif
_cod_data_source_block           compound-3_zam75
_cod_original_cell_volume        851.38(9)
_cod_database_code               4309175
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
Cu1 Cu 0.0000 0.5000 0.0000 0.02329(9) Uani 1 2 d S . .
O1 O 0.23885(14) 0.43505(14) 0.03957(11) 0.0338(3) Uani 1 1 d . . .
O2 O 0.46466(16) 0.55355(17) 0.20355(12) 0.0428(3) Uani 1 1 d . . .
O3 O 0.41674(18) 0.33916(16) 0.05192(15) 0.0510(4) Uani 1 1 d . . .
N1 N 0.18551(16) 0.73738(16) 0.05276(11) 0.0245(3) Uani 1 1 d . . .
N3 N -0.01092(16) 0.55005(15) 0.17607(11) 0.0239(3) Uani 1 1 d . . .
N4 N 0.37522(16) 0.44218(17) 0.09912(13) 0.0291(3) Uani 1 1 d . . .
C1 C 0.1332(2) 0.8411(2) 0.03856(14) 0.0281(3) Uani 1 1 d . . .
H1 H 0.0102 0.8011 0.0031 0.034 Uiso 1 1 calc R . .
C2 C 0.2512(2) 1.0035(2) 0.07349(15) 0.0314(3) Uani 1 1 d . . .
H2 H 0.2100 1.0725 0.0599 0.038 Uiso 1 1 calc R . .
C3 C 0.4296(2) 1.0643(2) 0.12831(15) 0.0298(3) Uani 1 1 d . . .
H3 H 0.5125 1.1760 0.1543 0.036 Uiso 1 1 calc R . .
C4 C 0.4861(2) 0.95922(19) 0.14488(14) 0.0266(3) Uani 1 1 d . . .
C5 C 0.35979(19) 0.79616(19) 0.10439(14) 0.0261(3) Uani 1 1 d . . .
H5 H 0.3983 0.7237 0.1136 0.031 Uiso 1 1 calc R . .
C6 C 0.6693(2) 1.0128(2) 0.20002(15) 0.0305(3) Uani 1 1 d . . .
C7 C 0.8213(2) 1.0529(2) 0.24180(15) 0.0312(3) Uani 1 1 d . . .
C8 C 1.0042(2) 1.10222(19) 0.29388(14) 0.0291(3) Uani 1 1 d . . .
C9 C 1.0471(2) 1.0096(2) 0.34494(18) 0.0399(4) Uani 1 1 d . . .
H9 H 0.9553 0.9110 0.3413 0.048 Uiso 1 1 calc R . .
C10 C 1.2231(2) 1.0613(2) 0.40075(18) 0.0403(4) Uani 1 1 d . . .
H10 H 1.2512 0.9984 0.4359 0.048 Uiso 1 1 calc R . .
C11 C 1.3596(2) 1.2053(2) 0.40576(14) 0.0301(3) Uani 1 1 d . . .
C12 C 1.3172(2) 1.2966(2) 0.35364(15) 0.0295(3) Uani 1 1 d . . .
H12 H 1.4092 1.3944 0.3562 0.035 Uiso 1 1 calc R . .
C13 C 1.1409(2) 1.2449(2) 0.29807(15) 0.0292(3) Uani 1 1 d . . .
H13 H 1.1130 1.3074 0.2624 0.035 Uiso 1 1 calc R . .
C14 C 0.4588(2) 0.7406(2) 0.53231(14) 0.0315(3) Uani 1 1 d . . .
C15 C 0.3110(2) 0.6974(2) 0.47590(14) 0.0297(3) Uani 1 1 d . . .
C16 C 0.13659(19) 0.60307(18) 0.26594(14) 0.0251(3) Uani 1 1 d . . .
H16 H 0.2410 0.6145 0.2437 0.030 Uiso 1 1 calc R . .
C17 C 0.14403(19) 0.64201(18) 0.38985(14) 0.0252(3) Uani 1 1 d . . .
C18 C -0.0099(2) 0.6249(2) 0.42209(15) 0.0311(3) Uani 1 1 d . . .
H18 H -0.0105 0.6494 0.5058 0.037 Uiso 1 1 calc R . .
C19 C -0.1614(2) 0.5715(2) 0.32934(16) 0.0330(4) Uani 1 1 d . . .
H19 H -0.2675 0.5597 0.3491 0.040 Uiso 1 1 calc R . .
C20 C -0.1585(2) 0.5353(2) 0.20824(15) 0.0284(3) Uani 1 1 d . . .
H20 H -0.2634 0.4989 0.1456 0.034 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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 '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
N3 Cu1 N3 180.00(8) . 2_565 ?
N3 Cu1 N1 89.28(5) . . ?
N3 Cu1 N1 90.72(5) 2_565 . ?
N3 Cu1 N1 90.72(5) . 2_565 ?
N3 Cu1 N1 89.28(5) 2_565 2_565 ?
N1 Cu1 N1 180.00(7) . 2_565 ?
C5 N1 C1 118.02(13) . . ?
C5 N1 Cu1 122.35(10) . . ?
C1 N1 Cu1 119.61(10) . . ?
C16 N3 C20 118.19(13) . . ?
C16 N3 Cu1 118.51(10) . . ?
C20 N3 Cu1 123.29(10) . . ?
O3 N4 O2 121.55(14) . . ?
O3 N4 O1 119.32(14) . . ?
O2 N4 O1 119.14(14) . . ?
N1 C1 C2 122.64(14) . . ?
C3 C2 C1 119.34(15) . . ?
C2 C3 C4 118.85(15) . . ?
C3 C4 C5 118.50(14) . . ?
C3 C4 C6 122.22(14) . . ?
C5 C4 C6 119.28(14) . . ?
N1 C5 C4 122.62(14) . . ?
C7 C6 C4 177.46(18) . . ?
C6 C7 C8 179.18(19) . . ?
C13 C8 C9 119.06(15) . . ?
C13 C8 C7 120.71(15) . . ?
C9 C8 C7 120.20(15) . . ?
C10 C9 C8 120.21(16) . . ?
C9 C10 C11 120.47(16) . . ?
C12 C11 C10 119.39(15) . . ?
C12 C11 C14 121.06(15) . 2_776 ?
C10 C11 C14 119.52(15) . 2_776 ?
C13 C12 C11 120.05(15) . . ?
C12 C13 C8 120.81(15) . . ?
C15 C14 C11 176.57(18) . 2_776 ?
C14 C15 C17 170.20(17) . . ?
N3 C16 C17 123.21(14) . . ?
C16 C17 C18 118.18(13) . . ?
C16 C17 C15 117.12(14) . . ?
C18 C17 C15 124.71(14) . . ?
C19 C18 C17 118.50(15) . . ?
C20 C19 C18 119.97(15) . . ?
N3 C20 C19 121.95(14) . . ?
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
Cu1 N3 2.0217(13) . ?
Cu1 N3 2.0217(13) 2_565 ?
Cu1 N1 2.0437(13) . ?
Cu1 N1 2.0437(13) 2_565 ?
O1 N4 1.2689(16) . ?
O2 N4 1.2447(19) . ?
O3 N4 1.2356(18) . ?
N1 C5 1.3456(18) . ?
N1 C1 1.348(2) . ?
N3 C16 1.3420(18) . ?
N3 C20 1.3487(19) . ?
C1 C2 1.382(2) . ?
C2 C3 1.381(2) . ?
C3 C4 1.394(2) . ?
C4 C5 1.395(2) . ?
C4 C6 1.435(2) . ?
C6 C7 1.192(2) . ?
C7 C8 1.436(2) . ?
C8 C13 1.392(2) . ?
C8 C9 1.401(2) . ?
C9 C10 1.385(2) . ?
C10 C11 1.397(3) . ?
C11 C12 1.394(2) . ?
C11 C14 1.440(2) 2_776 ?
C12 C13 1.386(2) . ?
C14 C15 1.194(2) . ?
C14 C11 1.440(2) 2_776 ?
C15 C17 1.436(2) . ?
C16 C17 1.388(2) . ?
C17 C18 1.397(2) . ?
C18 C19 1.384(2) . ?
C19 C20 1.379(2) . ?
