#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:21:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179661 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/14/4511488.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_4511488
loop_
_publ_author_name
'Hu, Sheng'
'Zhou, Ai-Ju'
'Zhang, Yue-Hua'
'Ding, Shu'
'Tong, Ming-Liang'
_publ_section_title
;
 1D Tubular Chains and 3D Polycatenane Frameworks Constructed with
 Cu2X2Dimers (X = Br-, I-, CN-) and Flexible Dipyridyl Spacers
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2543
_journal_paper_doi               10.1021/cg060370k
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C33 H36 Cu2 I2 N4'
_chemical_formula_weight         869.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.335(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.072(2)
_cell_length_b                   13.100(2)
_cell_length_c                   8.4752(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1779.3(4)
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_collection       'SMART, 1998.'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_method       'phi and omega scans'
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2691
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.956
_exptl_absorpt_correction_T_max  0.8426
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1554
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0650P)²+3.2775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                1295
_reflns_number_total             1554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060370ksi20060904_105804.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        1779.3(5)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4511488
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
I1 I 0.59934(3) -0.5000 -0.18217(6) 0.0603(2) Uani 1 2 d S
Cu1 Cu 0.56237(6) -0.5000 0.11470(12) 0.0544(3) Uani 1 2 d S
N1 N 0.6109(3) -0.3702(3) 0.2202(5) 0.0505(10) Uani 1 1 d .
C1 C 0.6751(4) -0.3191(5) 0.1679(8) 0.0718(17) Uani 1 1 d .
H1A H 0.6990 -0.3438 0.0789 0.086 Uiso 1 1 calc R
C2 C 0.7082(4) -0.2313(5) 0.2388(8) 0.0725(18) Uani 1 1 d .
H2A H 0.7533 -0.1991 0.1974 0.087 Uiso 1 1 calc R
C3 C 0.6751(3) -0.1919(4) 0.3685(7) 0.0539(13) Uani 1 1 d .
C4 C 0.6107(4) -0.2460(5) 0.4257(8) 0.0710(17) Uani 1 1 d .
H4A H 0.5869 -0.2238 0.5163 0.085 Uiso 1 1 calc R
C5 C 0.5812(4) -0.3336(5) 0.3490(8) 0.0696(17) Uani 1 1 d .
H5A H 0.5376 -0.3687 0.3911 0.084 Uiso 1 1 calc R
C6 C 0.7065(4) -0.0955(4) 0.4468(8) 0.0644(16) Uani 1 1 d .
H6A H 0.7667 -0.0932 0.4452 0.077 Uiso 1 1 calc R
H6B H 0.6933 -0.0965 0.5566 0.077 Uiso 1 1 calc R
C7 C 0.6700(6) 0.0000 0.3691(11) 0.064(2) Uani 1 2 d S
H7A H 0.6809 0.0000 0.2581 0.077 Uiso 1 2 calc SR
H7B H 0.6100 0.0000 0.3756 0.077 Uiso 1 2 calc SR
C8 C 0.5000 0.0537(4) 0.0000 0.186(7) Uiso 0.50 2 d SPD
C9 C 0.4394(16) 0.0000 0.073(4) 0.186(7) Uiso 0.50 2 d SPD
C10 C 0.4481(19) -0.1080(9) 0.087(3) 0.186(7) Uiso 0.50 1 d PD
C11 C 0.5000 -0.168(2) 0.0000 0.186(7) Uiso 0.50 2 d SPD
C12 C 0.4026(15) -0.0535(4) 0.191(2) 0.186(7) Uiso 0.50 1 d PD
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
Cu1 I1 Cu1 60.46(4) . 5_645
N1 Cu1 N1 112.3(2) . 6_545
N1 Cu1 I1 108.16(12) . .
N1 Cu1 I1 108.16(12) 6_545 .
N1 Cu1 Cu1 123.72(12) . 5_645
N1 Cu1 Cu1 123.72(12) 6_545 5_645
I1 Cu1 Cu1 61.14(4) . 5_645
N1 Cu1 I1 104.38(13) . 5_645
N1 Cu1 I1 104.38(13) 6_545 5_645
I1 Cu1 I1 119.54(4) . 5_645
Cu1 Cu1 I1 58.40(4) 5_645 5_645
C5 N1 C1 115.6(5) . .
C5 N1 Cu1 121.0(4) . .
C1 N1 Cu1 123.4(4) . .
N1 C1 C2 123.7(6) . .
N1 C1 H1A 118.2 . .
C2 C1 H1A 118.2 . .
C3 C2 C1 120.3(6) . .
C3 C2 H2A 119.8 . .
C1 C2 H2A 119.8 . .
C2 C3 C4 116.2(5) . .
C2 C3 C6 122.7(5) . .
C4 C3 C6 121.1(5) . .
C3 C4 C5 120.2(6) . .
C3 C4 H4A 119.9 . .
C5 C4 H4A 119.9 . .
N1 C5 C4 123.9(6) . .
N1 C5 H5A 118.0 . .
C4 C5 H5A 118.0 . .
C3 C6 C7 113.5(5) . .
C3 C6 H6A 108.9 . .
C7 C6 H6A 108.9 . .
C3 C6 H6B 108.9 . .
C7 C6 H6B 108.9 . .
H6A C6 H6B 107.7 . .
C6 C7 C6 111.7(7) 6 .
C6 C7 H7A 109.3 6 .
C6 C7 H7A 109.3 . .
C6 C7 H7B 109.3 6 .
C6 C7 H7B 109.3 . .
H7A C7 H7B 107.9 . .
C10 C8 C10 116.7(10) 6 5_655
C10 C8 C9 62.7(7) 6 .
C10 C8 C9 173(2) 5_655 .
C10 C8 C9 173(2) 6 5_655
C10 C8 C9 62.7(7) 5_655 5_655
C9 C8 C9 118.9(7) . 5_655
C10 C8 C8 121.7(5) 6 6
C10 C8 C8 121.7(5) 5_655 6
C9 C8 C8 59.5(3) . 6
C9 C8 C8 59.5(3) 5_655 6
C10 C8 C11 58.3(5) 6 5_655
C10 C8 C11 58.3(5) 5_655 5_655
C9 C8 C11 120.5(3) . 5_655
C9 C8 C11 120.5(3) 5_655 5_655
C8 C8 C11 180.0 6 5_655
C8 C9 C8 61.1(7) . 6
C8 C9 C12 114.6(13) . 6
C8 C9 C12 158(3) 6 6
C8 C9 C12 158(3) . .
C8 C9 C12 114.6(13) 6 .
C12 C9 C12 60.7(6) 6 .
C8 C9 C10 57.6(10) . 6
C8 C9 C10 118.2(14) 6 6
C12 C9 C10 59.0(5) 6 6
C12 C9 C10 119.2(9) . 6
C8 C9 C10 118.2(14) . .
C8 C9 C10 57.6(10) 6 .
C12 C9 C10 119.2(9) 6 .
C12 C9 C10 59.0(5) . .
C10 C9 C10 166(4) 6 .
C8 C10 C12 116.9(10) 6 .
C8 C10 C11 66.2(19) 6 .
C12 C10 C11 172(3) . .
C8 C10 C9 59.7(7) 6 .
C12 C10 C9 59.2(5) . .
C11 C10 C9 125(2) . .
C10 C11 C10 111(3) . 2_655
C10 C11 C8 55.5(16) . 6
C10 C11 C8 55.5(16) 2_655 6
C10 C12 C9 61.8(6) . .
C10 C12 C12 121.0(6) . 6
C9 C12 C12 59.6(3) . 6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.6287(12) .
I1 Cu1 2.7030(11) 5_645
Cu1 N1 2.048(4) .
Cu1 N1 2.048(4) 6_545
Cu1 Cu1 2.685(2) 5_645
Cu1 I1 2.7030(11) 5_645
N1 C5 1.315(7) .
N1 C1 1.333(7) .
C1 C2 1.385(8) .
C1 H1A 0.9300 .
C2 C3 1.359(8) .
C2 H2A 0.9300 .
C3 C4 1.373(8) .
C3 C6 1.496(7) .
C4 C5 1.386(8) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C6 C7 1.511(7) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C6 1.511(7) 6
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C10 1.35(2) 6
C8 C10 1.35(2) 5_655
C8 C9 1.385(10) .
C8 C9 1.385(10) 5_655
C8 C8 1.407(10) 6
C8 C11 1.50(3) 5_655
C9 C8 1.385(10) 6
C9 C12 1.388(7) 6
C9 C12 1.388(7) .
C9 C10 1.425(10) 6
C9 C10 1.425(10) .
C10 C8 1.35(2) 6
C10 C12 1.386(10) .
C10 C11 1.398(10) .
C11 C10 1.398(10) 2_655
C11 C8 1.50(3) 6
C12 C12 1.403(10) 6
