#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/60/7026076.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_7026076
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         'C10 H10 Cu3 N20 '
_chemical_formula_sum            'C10 H10 Cu3 N20'
_chemical_formula_weight         601.00
_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                 110.524(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9024(8)
_cell_length_b                   6.0183(2)
_cell_length_c                   14.8927(11)
_cell_measurement_reflns_used    6447
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.71
_cell_volume                     999.08(12)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6447
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    3.214
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.963
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details
w=1/[σ²(Fo²)+(0.0681P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                2211
_reflns_number_total             2889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00181c.txt
_cod_data_source_block           complex5
_cod_original_cell_volume        999.08(11)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C10 H10 Cu3 N20 '
_cod_database_code               7026076
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 0.19720(3) 0.29431(6) 0.13750(3) 0.01555(12) Uani 1 1 d .
Cu2 Cu 0.0000 0.0000 0.0000 0.01541(14) Uani 1 2 d S
N2 N 0.3058(2) 0.2802(4) 0.3357(2) 0.0146(5) Uani 1 1 d .
N10 N 0.3599(2) 0.3812(5) 0.1401(2) 0.0190(6) Uani 1 1 d .
N1 N 0.2332(2) 0.3853(4) 0.2753(2) 0.0181(5) Uani 1 1 d .
C1 C 0.4565(3) 0.2677(7) 0.1940(3) 0.0313(9) Uani 1 1 d .
H1 H 0.4460 0.1431 0.2271 0.038 Uiso 1 1 calc R
C5 C 0.3765(3) 0.5572(6) 0.0914(3) 0.0272(8) Uani 1 1 d .
H5 H 0.3098 0.6342 0.0518 0.033 Uiso 1 1 calc R
C4 C 0.4884(4) 0.6281(7) 0.0978(3) 0.0367(10) Uani 1 1 d .
H4 H 0.4970 0.7542 0.0647 0.044 Uiso 1 1 calc R
C3 C 0.5874(3) 0.5128(8) 0.1530(3) 0.0394(10) Uani 1 1 d .
H3 H 0.6639 0.5575 0.1574 0.047 Uiso 1 1 calc R
C2 C 0.5710(3) 0.3293(8) 0.2020(4) 0.0426(11) Uani 1 1 d .
H2 H 0.6367 0.2475 0.2401 0.051 Uiso 1 1 calc R
N4 N 0.0313(2) 0.1814(4) 0.1187(2) 0.0183(6) Uani 1 1 d .
N7 N 0.1555(2) 0.1396(4) 0.0116(2) 0.0182(6) Uani 1 1 d .
N3 N 0.3753(2) 0.1809(4) 0.3971(2) 0.0199(6) Uani 1 1 d .
N5 N -0.0460(2) 0.2934(5) 0.1316(2) 0.0219(6) Uani 1 1 d .
N8 N 0.2241(2) 0.0975(5) -0.0303(2) 0.0225(6) Uani 1 1 d .
N6 N -0.1186(3) 0.3966(6) 0.1454(3) 0.0411(9) Uani 1 1 d .
N9 N 0.2889(3) 0.0599(7) -0.0691(3) 0.0436(9) 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'
O O 0.0106 0.0060 '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'
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 93.46(11) . .
N10 Cu1 N4 172.04(12) . .
N7 Cu1 N4 78.65(11) . .
N10 Cu1 N1 92.92(11) . .
N7 Cu1 N1 167.51(11) . .
N4 Cu1 N1 94.64(11) . .
N10 Cu1 N3 91.32(10) . 2
N7 Cu1 N3 106.85(11) . 2
N4 Cu1 N3 91.98(10) . 2
N1 Cu1 N3 83.73(10) . 2
N10 Cu1 Cu2 132.30(8) . .
N7 Cu1 Cu2 39.22(7) . .
N4 Cu1 Cu2 39.74(8) . .
N1 Cu1 Cu2 132.28(8) . .
N3 Cu1 Cu2 105.89(7) 2 .
N7 Cu2 N7 180.0 . 3
N7 Cu2 N4 79.23(11) . .
N7 Cu2 N4 100.77(11) 3 .
N7 Cu2 N4 100.77(11) . 3
N7 Cu2 N4 79.23(11) 3 3
N4 Cu2 N4 180.0 . 3
N7 Cu2 N3 86.50(10) . 2_545
N7 Cu2 N3 93.50(10) 3 2_545
N4 Cu2 N3 89.50(10) . 2_545
N4 Cu2 N3 90.50(10) 3 2_545
N7 Cu2 N3 93.50(10) . 4_565
N7 Cu2 N3 86.50(10) 3 4_565
N4 Cu2 N3 90.50(10) . 4_565
N4 Cu2 N3 89.50(10) 3 4_565
N3 Cu2 N3 180.0 2_545 4_565
N7 Cu2 Cu1 140.54(8) . 3
N7 Cu2 Cu1 39.46(8) 3 3
N4 Cu2 Cu1 139.91(8) . 3
N4 Cu2 Cu1 40.08(8) 3 3
N3 Cu2 Cu1 96.46(6) 2_545 3
N3 Cu2 Cu1 83.54(6) 4_565 3
N7 Cu2 Cu1 39.46(8) . .
N7 Cu2 Cu1 140.54(8) 3 .
N4 Cu2 Cu1 40.09(8) . .
N4 Cu2 Cu1 139.92(8) 3 .
N3 Cu2 Cu1 83.54(6) 2_545 .
N3 Cu2 Cu1 96.46(6) 4_565 .
Cu1 Cu2 Cu1 180.0 3 .
N3 N2 N1 177.5(3) . .
C1 N10 C5 118.1(3) . .
C1 N10 Cu1 120.2(2) . .
C5 N10 Cu1 121.6(2) . .
N2 N1 Cu1 117.6(2) . .
N10 C1 C2 122.1(4) . .
N10 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
N10 C5 C4 122.3(3) . .
N10 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
C3 C4 C5 119.7(4) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C4 C3 C2 118.4(4) . .
C4 C3 H3 120.8 . .
C2 C3 H3 120.8 . .
C3 C2 C1 119.4(4) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
N5 N4 Cu2 122.0(2) . .
N5 N4 Cu1 123.6(2) . .
Cu2 N4 Cu1 100.18(13) . .
N8 N7 Cu2 129.9(2) . .
N8 N7 Cu1 126.1(2) . .
Cu2 N7 Cu1 101.32(13) . .
N2 N3 Cu1 102.7(2) . 2_545
N2 N3 Cu2 100.8(2) . 2
Cu1 N3 Cu2 155.68(13) 2_545 2
N6 N5 N4 178.7(4) . .
N9 N8 N7 179.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N10 1.994(3) .
Cu1 N7 1.994(3) .
Cu1 N4 2.013(3) .
Cu1 N1 2.020(3) .
Cu1 N3 2.472(3) 2
Cu1 Cu2 3.0772(4) .
Cu2 N7 1.984(3) .
Cu2 N7 1.984(3) 3
Cu2 N4 1.999(3) .
Cu2 N4 1.999(3) 3
Cu2 N3 2.578(3) 2_545
Cu2 N3 2.578(3) 4_565
Cu2 Cu1 3.0772(4) 3
N2 N3 1.161(4) .
N2 N1 1.188(4) .
N10 C1 1.336(5) .
N10 C5 1.336(4) .
C1 C2 1.378(5) .
C1 H1 0.9300 .
C5 C4 1.370(5) .
C5 H5 0.9300 .
C4 C3 1.365(6) .
C4 H4 0.9300 .
C3 C2 1.374(6) .
C3 H3 0.9300 .
C2 H2 0.9300 .
N4 N5 1.208(4) .
N7 N8 1.214(4) .
N3 Cu1 2.472(3) 2_545
N3 Cu2 2.578(3) 2
N5 N6 1.139(4) .
N8 N9 1.138(4) .
