#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:59:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179165 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/26/4312681.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_4312681
loop_
_publ_author_name
'En-Qing Gao'
'Shi-Qiang Bai'
'Chuan-Feng Wang'
'Yan-Feng Yue'
'Chun-Hua Yan'
_publ_contact_author_address
;
State Key Lab of Rare Earth Materials Chemistry and Applications & 
PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, 
College of Chemistry and Molecular Engineering, 
Peking University, 
Beijing 100871, 
China
;
_publ_contact_author_email       chyan@chem.pku.edu.cn
_publ_contact_author_fax         86-(10)-62754179
_publ_contact_author_name        'Prof. Chun-Hua Yan'
_publ_contact_author_phone       86-(10)-62754179
_publ_section_title
;
 Structural and Magnetic Properties of Three One-Dimensional Azido-Bridged
 Copper(II) and Manganese(II) Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8456
_journal_page_last               8464
_journal_paper_doi               10.1021/ic034618w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H11 Cu2 N15'
_chemical_formula_weight         468.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.8996(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3117(3)
_cell_length_b                   7.4950(2)
_cell_length_c                   20.9408(7)
_cell_measurement_reflns_used    30771
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1754.01(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_diffrn_measurement_method       CCD
_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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.1069
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26386
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.457
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.095
_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     232
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_gt           0.0620
_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)+(0.0840P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                1813
_reflns_number_total             3998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034618wsi20030604_105834_3.cif
_cod_data_source_block           Complex2
_cod_database_code               4312681
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.90519(6) 0.57285(10) 0.10114(4) 0.0590(3) Uani 1 1 d . . .
Cu2 Cu 0.99352(6) 0.77845(10) -0.01202(4) 0.0597(3) Uani 1 1 d . . .
N2 N 0.7513(5) 0.5673(8) 0.1350(3) 0.0647(14) Uani 1 1 d . . .
N3 N 0.7426(5) 0.6305(8) 0.1934(3) 0.0754(16) Uani 1 1 d . . .
N4 N 0.8460(5) 0.7311(7) 0.0272(3) 0.0633(14) Uani 1 1 d . . .
N5 N 0.7509(6) 0.7961(9) 0.0103(3) 0.0809(17) Uani 1 1 d . . .
N6 N 0.6619(7) 0.8589(13) -0.0068(4) 0.133(3) Uani 1 1 d . . .
N7 N 1.0544(5) 0.6068(6) 0.0613(3) 0.0598(13) Uani 1 1 d . . .
N8 N 1.1600(6) 0.5973(7) 0.0833(3) 0.0707(15) Uani 1 1 d . . .
N9 N 1.2584(6) 0.5868(11) 0.1029(4) 0.113(3) Uani 1 1 d . . .
N10 N 0.9198(5) 0.9740(7) -0.0661(3) 0.0747(16) Uani 1 1 d . . .
N11 N 0.9328(5) 1.0080(7) -0.1207(4) 0.0658(15) Uani 1 1 d . . .
N12 N 0.9417(6) 1.0487(9) -0.1718(3) 0.091(2) Uani 1 1 d . . .
N13 N 0.8806(5) 0.2855(7) 0.0632(3) 0.0693(15) Uani 1 1 d . . .
N14 N 0.8333(5) 0.1848(8) 0.0951(3) 0.0761(17) Uani 1 1 d . . .
N15 N 0.7837(6) 0.0966(10) 0.1259(4) 0.105(2) Uani 1 1 d . . .
N1 N 0.9866(3) 0.5114(5) 0.19060(18) 0.0680(16) Uani 1 1 d G . .
C1 C 1.0867(4) 0.4016(6) 0.2005(2) 0.0734(19) Uani 1 1 d G . .
H1A H 1.1136 0.3473 0.1655 0.088 Uiso 1 1 calc R . .
C2 C 1.1467(4) 0.3729(7) 0.2627(3) 0.096(3) Uani 1 1 d G . .
H2A H 1.2137 0.2994 0.2694 0.116 Uiso 1 1 calc R . .
C3 C 1.1065(5) 0.4540(9) 0.3151(2) 0.182(6) Uani 1 1 d G . .
H3A H 1.1467 0.4347 0.3567 0.219 Uiso 1 1 calc R . .
C4 C 1.0063(5) 0.5638(8) 0.3052(2) 0.132(4) Uani 1 1 d G . .
H4A H 0.9795 0.6181 0.3402 0.159 Uiso 1 1 calc R . .
C5 C 0.9464(4) 0.5925(6) 0.2429(2) 0.0658(19) Uani 1 1 d G . .
C6 C 0.8486(7) 0.7088(9) 0.2314(4) 0.079(2) Uani 1 1 d . . .
H6A H 0.8718 0.8132 0.2089 0.095 Uiso 1 1 calc R . .
H6B H 0.8287 0.7482 0.2725 0.095 Uiso 1 1 calc R . .
C7 C 0.6290(8) 0.6265(11) 0.2106(5) 0.100(3) Uani 1 1 d . . .
H7A H 0.6076 0.6633 0.2497 0.120 Uiso 1 1 calc R . .
C8 C 0.5502(7) 0.5533(13) 0.1554(8) 0.158(6) Uani 1 1 d . . .
H8A H 0.4681 0.5328 0.1493 0.190 Uiso 1 1 calc R . .
C9 C 0.6442(11) 0.5191(13) 0.1091(4) 0.108(4) Uani 1 1 d . . .
C10 C 0.6168(11) 0.435(2) 0.0538(9) 0.258(11) Uani 1 1 d . . .
H10A H 0.6862 0.4284 0.0327 0.387 Uiso 1 1 calc R . .
H10B H 0.5545 0.4989 0.0268 0.387 Uiso 1 1 calc R . .
H10C H 0.5897 0.3169 0.0614 0.387 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'
Cu Cu 0.3201 1.2651 '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
N2 Cu1 N4 94.7(2) . . ?
N2 Cu1 N1 87.9(2) . . ?
N4 Cu1 N1 156.3(2) . . ?
N2 Cu1 N7 172.9(2) . . ?
N4 Cu1 N7 78.7(2) . . ?
N1 Cu1 N7 97.06(19) . . ?
N2 Cu1 N13 92.2(2) . . ?
N4 Cu1 N13 106.5(2) . . ?
N1 Cu1 N13 96.94(19) . . ?
N7 Cu1 N13 92.28(19) . . ?
N10 Cu2 N13 98.4(3) . 3_765 ?
N10 Cu2 N4 93.6(2) . . ?
N13 Cu2 N4 154.0(2) 3_765 . ?
N10 Cu2 N7 166.3(2) . . ?
N13 Cu2 N7 93.9(2) 3_765 . ?
N4 Cu2 N7 77.6(2) . . ?
N10 Cu2 N10 85.1(2) . 3_775 ?
N13 Cu2 N10 106.6(2) 3_765 3_775 ?
N4 Cu2 N10 97.3(2) . 3_775 ?
N7 Cu2 N10 85.68(19) . 3_775 ?
C9 N2 N3 106.6(7) . . ?
C9 N2 Cu1 132.2(6) . . ?
N3 N2 Cu1 121.1(4) . . ?
N2 N3 C7 115.7(7) . . ?
N2 N3 C6 118.2(6) . . ?
C7 N3 C6 125.8(8) . . ?
N5 N4 Cu1 131.4(5) . . ?
N5 N4 Cu2 125.4(5) . . ?
Cu1 N4 Cu2 103.0(2) . . ?
N6 N5 N4 178.6(8) . . ?
N8 N7 Cu1 132.5(5) . . ?
N8 N7 Cu2 121.4(4) . . ?
Cu1 N7 Cu2 100.7(2) . . ?
N9 N8 N7 178.9(8) . . ?
N11 N10 Cu2 127.2(5) . . ?
N12 N11 N10 176.2(8) . . ?
N14 N13 Cu2 125.3(5) . 3_765 ?
N14 N13 Cu1 116.2(4) . . ?
Cu2 N13 Cu1 110.9(2) 3_765 . ?
N15 N14 N13 176.0(8) . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Cu1 121.3(3) . . ?
C5 N1 Cu1 118.5(3) . . ?
C2 C1 N1 120.0 . . ?
C1 C2 C3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 121.1(5) . . ?
N1 C5 C6 118.8(5) . . ?
C5 C6 N3 113.9(6) . . ?
N3 C7 C8 106.3(8) . . ?
C7 C8 C9 99.4(6) . . ?
N2 C9 C10 125.4(13) . . ?
N2 C9 C8 111.9(7) . . ?
C10 C9 C8 122.3(13) . . ?
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 N2 1.979(5) . ?
Cu1 N4 1.982(5) . ?
Cu1 N1 2.009(3) . ?
Cu1 N7 2.011(5) . ?
Cu1 N13 2.297(5) . ?
Cu2 N10 1.958(6) . ?
Cu2 N13 1.970(5) 3_765 ?
Cu2 N4 2.002(5) . ?
Cu2 N7 2.040(5) . ?
Cu2 N10 2.566(6) 3_775 ?
N2 C9 1.300(12) . ?
N2 N3 1.331(7) . ?
N3 C7 1.386(8) . ?
N3 C6 1.456(9) . ?
N4 N5 1.185(8) . ?
N5 N6 1.119(8) . ?
N7 N8 1.214(7) . ?
N8 N9 1.128(7) . ?
N10 N11 1.203(8) . ?
N11 N12 1.131(8) . ?
N13 N14 1.189(7) . ?
N13 Cu2 1.970(5) 3_765 ?
N14 N15 1.131(8) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.399(7) . ?
C7 C8 1.454(15) . ?
C8 C9 1.567(15) . ?
C9 C10 1.31(2) . ?
