#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:55:57 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180115 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/13/7101303.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_7101303
loop_
_publ_author_name
D.Ray
G.Aromi
P.K.Nanda
_publ_section_title
;
Tetranuclear Cu(II) complex supported by a central μ4-1,1,3,3 azide
bridge
;
_journal_issue                   30
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b604502b
_journal_year                    2006
_chemical_formula_sum            'C60 H98 Cl Cu4 N11 O22'
_chemical_formula_weight         1614.52
_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                 103.600(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.7689(4)
_cell_length_b                   18.0119(8)
_cell_length_c                   13.5174(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     3495.0(3)
_computing_cell_refinement       cad4
_computing_data_collection       cad4
_computing_data_reduction        cad4
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  cad4
_diffrn_measurement_method       /W-scan
_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  0.1559
_diffrn_reflns_av_sigmaI/netI    0.1418
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5955
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         25
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1459
_refine_ls_R_factor_gt           0.0810
_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)+(0.1232P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2343
_reflns_number_gt                1620
_reflns_number_total             3079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604502b.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7101303
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
Cu1 Cu 0.18554(6) 0.41237(5) 0.10904(6) 0.0553(4) Uani 1 1 d .
O1 O 0.2618(5) 0.5000 0.0910(4) 0.0497(15) Uani 1 2 d S
O2 O 0.1662(4) 0.3905(3) -0.0303(4) 0.0694(15) Uani 1 1 d .
O3A O 0.2485(12) 0.5000 0.8689(11) 0.058(4) Uiso 0.50 2 d SP
O3B O 0.2078(15) 0.5000 0.8506(14) 0.079(6) Uiso 0.50 2 d SP
O4A O 0.2870(19) 0.6352(16) 0.6003(17) 0.176(9) Uiso 0.50 1 d P
O4B O 0.2196(18) 0.6360(15) 0.5920(16) 0.161(8) Uiso 0.50 1 d P
O5 O 0.0279(17) 0.5354(15) 0.5417(16) 0.199(11) Uiso 0.50 1 d P
O6A O 0.461(2) 0.677(2) 0.509(3) 0.243(16) Uiso 0.50 1 d P
O6B O 0.409(2) 0.6697(19) 0.545(2) 0.194(10) Uiso 0.50 1 d P
O7A O 0.129(3) 0.262(3) 0.503(3) 0.30(2) Uiso 0.50 1 d P
O7B O 0.090(3) 0.324(3) 0.496(3) 0.32(2) Uiso 0.50 1 d P
N1 N 0.1679(4) 0.3098(3) 0.1456(5) 0.0569(15) Uani 1 1 d .
N2 N 0.2067(4) 0.4361(3) 0.2627(4) 0.0535(14) Uani 1 1 d .
N3 N 0.0591(7) 0.5000 0.0711(8) 0.071(2) Uani 1 2 d S
N4 N 0.0000 0.5000 0.0000 0.054(3) Uani 1 4 d S
C1 C 0.1322(5) 0.3284(4) -0.0763(6) 0.0591(19) Uani 1 1 d .
C2 C 0.1080(6) 0.3297(5) -0.1804(6) 0.068(2) Uani 1 1 d .
H2 H 0.1116 0.3744 -0.2138 0.082 Uiso 1 1 calc R
C3 C 0.0786(5) 0.2671(5) -0.2375(6) 0.067(2) Uani 1 1 d .
H3 H 0.0626 0.2700 -0.3082 0.081 Uiso 1 1 calc R
C4 C 0.0730(6) 0.2009(6) -0.1906(7) 0.082(3) Uani 1 1 d .
H4 H 0.0538 0.1583 -0.2287 0.098 Uiso 1 1 calc R
C5 C 0.0961(6) 0.1981(5) -0.0862(7) 0.075(2) Uani 1 1 d .
H5 H 0.0905 0.1532 -0.0542 0.090 Uiso 1 1 calc R
C6 C 0.1285(5) 0.2618(4) -0.0246(5) 0.0527(17) Uani 1 1 d .
C7 C 0.1480(5) 0.2521(4) 0.0857(6) 0.0589(18) Uani 1 1 d .
C8 C 0.1471(6) 0.1766(4) 0.1282(7) 0.075(2) Uani 1 1 d .
H8A H 0.2032 0.1510 0.1245 0.112 Uiso 1 1 calc R
H8B H 0.0942 0.1498 0.0897 0.112 Uiso 1 1 calc R
H8C H 0.1431 0.1799 0.1979 0.112 Uiso 1 1 calc R
C9 C 0.1843(6) 0.3010(5) 0.2546(6) 0.068(2) Uani 1 1 d .
H9A H 0.2167 0.2546 0.2748 0.082 Uiso 1 1 calc R
H9B H 0.1252 0.2993 0.2741 0.082 Uiso 1 1 calc R
C10 C 0.2417(6) 0.3646(4) 0.3084(6) 0.0613(19) Uani 1 1 d .
H10A H 0.2399 0.3643 0.3797 0.074 Uiso 1 1 calc R
H10B H 0.3060 0.3583 0.3045 0.074 Uiso 1 1 calc R
C11 C 0.2703(7) 0.5000 0.3036(7) 0.055(2) Uani 1 2 d S
C12 C 0.2998(11) 0.5000 0.4208(10) 0.086(4) Uani 1 2 d S
H12A H 0.3352 0.4560 0.4438 0.128 Uiso 0.50 1 calc PR
H12B H 0.2453 0.5009 0.4480 0.128 Uiso 1 2 calc SR
H12C H 0.3372 0.5430 0.4437 0.128 Uiso 0.50 1 calc PR
C13 C 0.3561(7) 0.5000 0.2588(8) 0.057(3) Uani 1 2 d S
C14 C 0.4473(8) 0.5000 0.3224(8) 0.066(3) Uani 1 2 d S
H14 H 0.4554 0.5000 0.3927 0.079 Uiso 1 2 calc SR
C15 C 0.5233(9) 0.5000 0.2813(12) 0.077(3) Uani 1 2 d S
H15 H 0.5826 0.5000 0.3242 0.092 Uiso 1 2 calc SR
C16 C 0.5139(9) 0.5000 0.1791(11) 0.073(3) Uani 1 2 d S
H16 H 0.5665 0.5000 0.1525 0.088 Uiso 1 2 calc SR
C17 C 0.4239(8) 0.5000 0.1130(9) 0.066(3) Uani 1 2 d S
H17 H 0.4170 0.5000 0.0428 0.079 Uiso 1 2 calc SR
C18 C 0.3457(6) 0.5000 0.1543(7) 0.046(2) Uani 1 2 d S
C19 C 0.1157(6) 0.4579(5) 0.2886(6) 0.066(2) Uani 1 1 d .
H19A H 0.0629 0.4388 0.2381 0.079 Uiso 1 1 calc R
H19B H 0.1128 0.4388 0.3549 0.079 Uiso 1 1 calc R
Cl1 Cl 0.1961(4) 0.5000 0.6895(4) 0.0760(16) Uani 0.50 2 d SP
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'
Cl Cl 0.1484 0.1585 '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'
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
O2 Cu1 N1 93.3(2) . .
O2 Cu1 O1 90.0(2) . .
N1 Cu1 O1 154.0(3) . .
O2 Cu1 N2 179.8(2) . .
N1 Cu1 N2 86.5(2) . .
O1 Cu1 N2 90.2(2) . .
O2 Cu1 N3 89.8(3) . .
N1 Cu1 N3 122.2(3) . .
O1 Cu1 N3 83.5(2) . .
N2 Cu1 N3 90.3(3) . .
C18 O1 Cu1 113.0(3) . .
C18 O1 Cu1 113.0(3) . 6_565
Cu1 O1 Cu1 105.2(3) . 6_565
C1 O2 Cu1 126.9(5) . .
O3A O3B Cl1 105(3) . .
O5 O5 O5 90.000(2) 2_556 6_565
O5 O5 O5 46.0(15) 2_556 5_566
O5 O5 O5 44.0(15) 6_565 5_566
O6B O6A O6A 161(6) . 2_656
C7 N1 C9 120.2(7) . .
C7 N1 Cu1 128.4(5) . .
C9 N1 Cu1 111.3(5) . .
C10 N2 C11 112.9(6) . .
C10 N2 C19 111.9(6) . .
C11 N2 C19 103.1(6) . .
C10 N2 Cu1 101.3(4) . .
C11 N2 Cu1 117.4(5) . .
C19 N2 Cu1 110.6(4) . .
N4 N3 Cu1 125.7(4) . 6_565
N4 N3 Cu1 125.7(4) . .
Cu1 N3 Cu1 82.0(3) 6_565 .
N3 N4 N3 180 . 5_565
O2 C1 C2 116.6(7) . .
O2 C1 C6 123.2(7) . .
C2 C1 C6 119.9(7) . .
C1 C2 C3 122.2(8) . .
C4 C3 C2 120.1(8) . .
C3 C4 C5 118.9(8) . .
C4 C5 C6 122.5(9) . .
C1 C6 C5 116.4(7) . .
C1 C6 C7 126.3(7) . .
C5 C6 C7 117.1(7) . .
N1 C7 C6 119.9(7) . .
N1 C7 C8 120.8(7) . .
C6 C7 C8 119.3(7) . .
N1 C9 C10 110.4(6) . .
N2 C10 C9 111.2(6) . .
N2 C11 N2 99.7(8) . 6_565
N2 C11 C13 111.0(6) . .
N2 C11 C13 111.0(6) 6_565 .
N2 C11 C12 112.2(6) . .
N2 C11 C12 112.2(6) 6_565 .
C13 C11 C12 110.3(9) . .
C18 C13 C14 118.7(9) . .
C18 C13 C11 120.1(9) . .
C14 C13 C11 121.2(10) . .
C15 C14 C13 120.6(11) . .
C16 C15 C14 121.2(11) . .
C15 C16 C17 119.9(11) . .
C18 C17 C16 119.3(10) . .
O1 C18 C13 121.2(8) . .
O1 C18 C17 118.5(9) . .
C13 C18 C17 120.3(9) . .
C19 C19 N2 105.0(4) 6_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.880(5) .
Cu1 N1 1.945(6) .
Cu1 O1 1.987(4) .
Cu1 N2 2.072(6) .
Cu1 N3 2.406(8) .
O1 C18 1.330(11) .
O1 Cu1 1.987(4) 6_565
O2 C1 1.321(9) .
O3A O3B 0.59(2) .
O3B Cl1 2.144(19) .
O4A O4B 0.98(3) .
O5 O5 1.23(4) 2_556
O5 O5 1.28(5) 6_565
O5 O5 1.77(5) 5_566
O6A O6B 1.01(3) .
O6A O6A 1.23(7) 2_656
O7A O7B 1.24(7) .
N1 C7 1.309(9) .
N1 C9 1.445(9) .
N2 C10 1.469(10) .
N2 C11 1.506(9) .
N2 C19 1.519(9) .
N3 N4 1.136(11) .
N3 Cu1 2.406(8) 6_565
N4 N3 1.136(11) 5_565
C1 C2 1.369(10) .
C1 C6 1.396(10) .
C2 C3 1.377(11) .
C3 C4 1.362(13) .
C4 C5 1.374(12) .
C5 C6 1.432(11) .
C6 C7 1.461(10) .
C7 C8 1.478(10) .
C9 C10 1.506(11) .
C11 N2 1.506(9) 6_565
C11 C13 1.527(14) .
C11 C12 1.541(16) .
C13 C18 1.386(14) .
C13 C14 1.417(15) .
C14 C15 1.365(18) .
C15 C16 1.355(17) .
C16 C17 1.418(18) .
C17 C18 1.395(14) .
C19 C19 1.516(17) 6_565
