#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:22:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179966 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/60/7026075.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_7026075
loop_
_publ_author_name
'Sengupta, Oindrila'
'Gole, Bappaditya'
'Mukherjee, Sandip'
'Mukherjee, Partha Sarathi'
_publ_section_title
;
 A series of transition metal-azido extended complexes with various
 anionic and neutral co-ligands: synthesis, structure and their distinct
 magnetic behavior.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7451
_journal_page_last               7465
_journal_paper_doi               10.1039/c0dt00181c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C8 H8 Cu3 N22'
_chemical_formula_sum            'C8 H8 Cu3 N22'
_chemical_formula_weight         602.98
_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                 111.266(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9395(6)
_cell_length_b                   6.0952(3)
_cell_length_c                   15.2200(9)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.55
_cell_volume                     1032.19(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12068
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    3.113
_exptl_absorpt_correction_T_max  0.5475
_exptl_absorpt_correction_T_min  0.4760
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0324
_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)+(0.0352P)²+0.1007P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                2278
_reflns_number_total             3126
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c0dt00181c.txt
_cod_data_source_block           complex4
_cod_original_cell_volume        1032.19(9)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7026075
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
Cu1 Cu 0.19846(2) 0.21109(5) 0.13819(2) 0.02625(10) Uani 1 1 d .
Cu2 Cu 0.0000 0.5000 0.0000 0.02466(11) Uani 1 2 d S
N2 N 0.30587(17) 0.2248(3) 0.33408(14) 0.0250(4) Uani 1 1 d .
N3 N 0.37539(19) 0.3220(3) 0.39557(15) 0.0350(5) Uani 1 1 d .
N1 N 0.23301(17) 0.1221(3) 0.27344(13) 0.0286(4) Uani 1 1 d .
N7 N 0.15838(17) 0.3679(4) 0.01502(14) 0.0317(5) Uani 1 1 d .
N4 N 0.03114(17) 0.3219(3) 0.11649(14) 0.0270(4) Uani 1 1 d .
N8 N 0.22419(19) 0.4008(4) -0.02786(16) 0.0370(5) Uani 1 1 d .
N5 N -0.04519(19) 0.2128(4) 0.13073(17) 0.0373(5) Uani 1 1 d .
N10 N 0.36177(17) 0.1255(3) 0.14227(14) 0.0311(5) Uani 1 1 d .
N9 N 0.2873(3) 0.4298(6) -0.0672(3) 0.0814(10) Uani 1 1 d .
N6 N -0.1172(2) 0.1116(5) 0.1445(2) 0.0771(10) Uani 1 1 d .
C1 C 0.4574(3) 0.2407(6) 0.1935(2) 0.0545(9) Uani 1 1 d .
H1 H 0.4463 0.3635 0.2256 0.065 Uiso 1 1 calc R
C4 C 0.3782(3) -0.0485(5) 0.0953(2) 0.0454(7) Uani 1 1 d .
H4 H 0.3114 -0.1279 0.0578 0.054 Uiso 1 1 calc R
N11 N 0.5899(3) 0.0048(7) 0.1536(3) 0.0973(12) Uani 1 1 d .
C3 C 0.4908(3) -0.1151(6) 0.1001(3) 0.0609(9) Uani 1 1 d .
H3 H 0.4996 -0.2391 0.0676 0.073 Uiso 1 1 calc R
C2 C 0.5722(3) 0.1864(7) 0.2011(3) 0.0793(13) Uani 1 1 d .
H2 H 0.6371 0.2710 0.2378 0.095 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
N10 Cu1 N7 93.04(8) . .
N10 Cu1 N4 171.53(8) . .
N7 Cu1 N4 78.50(8) . .
N10 Cu1 N1 93.55(8) . .
N7 Cu1 N1 166.68(8) . .
N4 Cu1 N1 94.63(8) . .
N7 Cu2 N7 180.0 3_565 .
N7 Cu2 N4 79.33(8) 3_565 3_565
N7 Cu2 N4 100.67(8) . 3_565
N7 Cu2 N4 100.67(8) 3_565 .
N7 Cu2 N4 79.33(8) . .
N4 Cu2 N4 180.00(11) 3_565 .
N3 N2 N1 177.6(3) . .
N2 N1 Cu1 118.04(16) . .
N8 N7 Cu2 130.44(16) . .
N8 N7 Cu1 127.20(16) . .
Cu2 N7 Cu1 101.26(9) . .
N5 N4 Cu2 123.27(16) . .
N5 N4 Cu1 123.49(16) . .
Cu2 N4 Cu1 100.47(9) . .
N9 N8 N7 179.0(3) . .
N6 N5 N4 179.4(3) . .
C1 N10 C4 118.3(2) . .
C1 N10 Cu1 120.18(19) . .
C4 N10 Cu1 121.56(18) . .
N10 C1 C2 122.8(3) . .
N10 C4 C3 122.4(3) . .
C3 N11 C2 118.3(3) . .
N11 C3 C4 119.1(3) . .
C1 C2 N11 119.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N10 1.9975(19) .
Cu1 N7 2.002(2) .
Cu1 N4 2.0194(19) .
Cu1 N1 2.0214(19) .
Cu2 N7 1.9905(19) 3_565
Cu2 N7 1.9905(19) .
Cu2 N4 1.9954(19) 3_565
Cu2 N4 1.9954(19) .
N2 N3 1.163(3) .
N2 N1 1.191(3) .
N7 N8 1.206(3) .
N4 N5 1.209(3) .
N8 N9 1.134(3) .
N5 N6 1.138(3) .
N10 C1 1.326(4) .
N10 C4 1.333(3) .
C1 C2 1.373(4) .
C4 C3 1.380(4) .
N11 C3 1.378(5) .
N11 C2 1.380(5) .
