#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:53:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179352 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/49/4324941.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_4324941
loop_
_publ_author_name
'Mrinal Sarkar'
'Rodolphe Clérac'
'Corine Mathonière'
'Nigel G. R. Hearns'
'Valerio Bertolasi'
'Debashis Ray'
_publ_contact_author_address
; 
 Department of Chemistry 
 Indian Institute of Technology
 Kharagpur-721302
 India
;
_publ_contact_author_email       dray@chem.iitkgp.ernet.in
_publ_contact_author_fax         ' 913222-255303'
_publ_contact_author_name        'Prof. Debashis Ray'
_publ_contact_author_phone       03222-283324
_publ_section_title
;
 New Phenoxido-Bridged Quasi-Tetrahedral and Rhomboidal [Cu4] Compounds
 Bearing μ4-Oxido or μ1,1-Azido Ligands: Synthesis, Chemical Reactivity,
 and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3922
_journal_page_last               3933
_journal_paper_doi               10.1021/ic102226j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C70 H78 Cu4 N4 O11, 2(C H4 O)'
_chemical_formula_sum            'C72 H86 Cu4 N4 O13'
_chemical_formula_weight         1469.7
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.036(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0640(19)
_cell_length_b                   35.820(5)
_cell_length_c                   13.1134(17)
_cell_measurement_temperature    293(2)
_cell_volume                     6893.5(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49833
_diffrn_reflns_theta_full        29.74
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.282
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       Block
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.531
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         9743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1037P)²+7.3072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1805
_reflns_number_gt                6754
_reflns_number_total             9743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102226j_si_001_1.cif
_cod_data_source_block           drms1_0m-716092
_cod_original_cell_volume        6893.5(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4324941
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
O7 O 0.5000 0.12161(8) 0.7500 0.0282(6) Uani 1 2 d S
O1 O 0.5000 0.05272(9) 0.7500 0.0336(7) Uani 1 2 d S
O4 O 0.5000 0.19051(9) 0.7500 0.0359(7) Uani 1 2 d S
C2 C 0.4576(2) -0.00411(9) 0.8181(3) 0.0306(6) Uani 1 1 d .
C1 C 0.5000 0.01641(12) 0.7500 0.0279(9) Uani 1 2 d S
C6 C 0.4060(2) 0.01315(9) 0.8880(3) 0.0317(7) Uani 1 1 d .
H6 H 0.3776 -0.0033 0.9255 0.038 Uiso 1 1 calc R
C21 C 0.4182(2) 0.24738(10) 0.7124(3) 0.0356(7) Uani 1 1 d .
C25 C 0.3301(2) 0.23000(10) 0.6720(3) 0.0360(7) Uani 1 1 d .
H25 H 0.2805 0.2461 0.6555 0.043 Uiso 1 1 calc R
C20 C 0.5000 0.22708(12) 0.7500 0.0321(9) Uani 1 2 d S
O6 O 0.40079(16) 0.08028(8) 0.5353(2) 0.0429(6) Uani 1 1 d .
C3 C 0.4594(2) -0.04310(9) 0.8169(3) 0.0382(8) Uani 1 1 d .
H3 H 0.4320 -0.0560 0.8631 0.046 Uiso 1 1 calc R
C22 C 0.4207(3) 0.28641(10) 0.7153(3) 0.0453(9) Uani 1 1 d .
H22 H 0.3665 0.2995 0.6929 0.054 Uiso 1 1 calc R
C4 C 0.5000 -0.06323(13) 0.7500 0.0403(11) Uani 1 2 d S
C5 C 0.5000 -0.10514(16) 0.7500 0.068(2) Uani 1 2 d S
H5A H 0.5311 -0.1141 0.6984 0.102 Uiso 0.50 1 calc PR
H5B H 0.4383 -0.1141 0.7337 0.102 Uiso 0.50 1 calc PR
H5C H 0.5306 -0.1141 0.8179 0.102 Uiso 0.50 1 calc PR
C23 C 0.5000 0.30648(14) 0.7500 0.0479(13) Uani 1 2 d S
C24 C 0.5000 0.34887(17) 0.7500 0.081(3) Uani 1 2 d S
H24A H 0.5609 0.3578 0.7768 0.122 Uiso 0.50 1 calc PR
H24B H 0.4610 0.3578 0.7934 0.122 Uiso 0.50 1 calc PR
H24C H 0.4781 0.3578 0.6798 0.122 Uiso 0.50 1 calc PR
O2 O 0.41234(16) 0.12919(7) 0.9160(2) 0.0408(6) Uani 1 1 d .
O3 O 0.53627(18) 0.16505(8) 0.9677(2) 0.0482(7) Uani 1 1 d .
C13 C 0.4555(2) 0.15681(10) 0.9638(3) 0.0369(7) Uani 1 1 d .
C14 C 0.4004(2) 0.18150(10) 1.0194(3) 0.0386(8) Uani 1 1 d .
C19 C 0.3069(3) 0.17828(12) 0.9984(4) 0.0522(10) Uani 1 1 d .
H19 H 0.2781 0.1611 0.9487 0.063 Uiso 1 1 calc R
C15 C 0.4408(3) 0.20696(13) 1.0934(4) 0.0612(12) Uani 1 1 d .
H15 H 0.5038 0.2098 1.1081 0.073 Uiso 1 1 calc R
C18 C 0.2547(3) 0.20017(14) 1.0498(4) 0.0667(13) Uani 1 1 d .
H18 H 0.1917 0.1977 1.0346 0.080 Uiso 1 1 calc R
C17 C 0.2969(4) 0.22530(14) 1.1229(4) 0.0693(14) Uani 1 1 d .
H17 H 0.2623 0.2404 1.1568 0.083 Uiso 1 1 calc R
C16 C 0.3900(4) 0.22853(15) 1.1468(5) 0.0755(16) Uani 1 1 d .
H16 H 0.4188 0.2451 1.1984 0.091 Uiso 1 1 calc R
O8 O 0.6949(3) 0.18742(13) 1.1100(3) 0.0888(12) Uani 1 1 d .
C39 C 0.7036(5) 0.15554(19) 1.1725(7) 0.103(2) Uani 1 1 d .
Cu1 Cu 0.46066(2) 0.088417(10) 0.84582(3) 0.02807(12) Uani 1 1 d .
Cu2 Cu 0.40595(2) 0.154958(11) 0.68155(3) 0.03001(12) Uani 1 1 d .
N1 N 0.39500(17) 0.04801(7) 0.9041(2) 0.0303(6) Uani 1 1 d .
C32 C 0.3308(2) 0.08935(8) 0.5590(3) 0.0263(6) Uani 1 1 d .
O5 O 0.32118(16) 0.11467(7) 0.6271(2) 0.0411(6) Uani 1 1 d .
N2 N 0.31227(17) 0.19516(8) 0.6561(2) 0.0314(6) Uani 1 1 d .
C26 C 0.2153(2) 0.18404(10) 0.6183(3) 0.0342(7) Uani 1 1 d .
H26 H 0.2135 0.1650 0.5642 0.041 Uiso 1 1 calc R
C7 C 0.3306(2) 0.05873(10) 0.9698(3) 0.0347(7) Uani 1 1 d .
H7 H 0.3577 0.0800 1.0126 0.042 Uiso 1 1 calc R
C33 C 0.2407(2) 0.07078(9) 0.5093(3) 0.0373(7) Uani 1 1 d .
C12 C 0.3087(2) 0.02945(11) 1.0444(3) 0.0430(8) Uani 1 1 d .
H12A H 0.2779 0.0085 1.0049 0.052 Uiso 1 1 calc R
H12B H 0.3647 0.0204 1.0896 0.052 Uiso 1 1 calc R
C34 C 0.2230(3) 0.06175(12) 0.4044(3) 0.0474(9) Uani 1 1 d .
H34 H 0.2666 0.0664 0.3658 0.057 Uiso 1 1 calc R
C8 C 0.2430(3) 0.07267(13) 0.8980(4) 0.0524(10) Uani 1 1 d .
H8A H 0.2137 0.0523 0.8542 0.063 Uiso 1 1 calc R
H8B H 0.2571 0.0921 0.8527 0.063 Uiso 1 1 calc R
C31 C 0.1488(2) 0.21431(12) 0.5705(3) 0.0463(9) Uani 1 1 d .
H31A H 0.1693 0.2263 0.5135 0.056 Uiso 1 1 calc R
H31B H 0.1453 0.2331 0.6227 0.056 Uiso 1 1 calc R
C28 C 0.0881(3) 0.14838(13) 0.6673(4) 0.0583(11) Uani 1 1 d .
H28A H 0.0917 0.1287 0.6177 0.070 Uiso 1 1 calc R
H28B H 0.0671 0.1374 0.7253 0.070 Uiso 1 1 calc R
C27 C 0.1830(2) 0.16539(11) 0.7078(3) 0.0432(8) Uani 1 1 d .
H27A H 0.1807 0.1837 0.7618 0.052 Uiso 1 1 calc R
H27B H 0.2257 0.1460 0.7384 0.052 Uiso 1 1 calc R
C9 C 0.1774(4) 0.08816(15) 0.9624(5) 0.0752(16) Uani 1 1 d .
H9A H 0.2032 0.1107 0.9981 0.090 Uiso 1 1 calc R
H9B H 0.1201 0.0947 0.9154 0.090 Uiso 1 1 calc R
C30 C 0.0548(3) 0.19675(14) 0.5294(4) 0.0588(11) Uani 1 1 d .
H30A H 0.0118 0.2160 0.4987 0.071 Uiso 1 1 calc R
H30B H 0.0583 0.1788 0.4750 0.071 Uiso 1 1 calc R
C10 C 0.1597(3) 0.06018(15) 1.0424(5) 0.0683(14) Uani 1 1 d .
H10A H 0.1234 0.0718 1.0860 0.082 Uiso 1 1 calc R
H10B H 0.1255 0.0392 1.0067 0.082 Uiso 1 1 calc R
C38 C 0.1764(3) 0.06332(12) 0.5659(4) 0.0527(10) Uani 1 1 d .
H38 H 0.1877 0.0699 0.6363 0.063 Uiso 1 1 calc R
C35 C 0.1402(3) 0.04565(15) 0.3562(4) 0.0655(13) Uani 1 1 d .
H35 H 0.1277 0.0402 0.2850 0.079 Uiso 1 1 calc R
C29 C 0.0212(3) 0.17752(15) 0.6151(4) 0.0632(12) Uani 1 1 d .
H29A H -0.0371 0.1658 0.5862 0.076 Uiso 1 1 calc R
H29B H 0.0124 0.1958 0.6666 0.076 Uiso 1 1 calc R
C11 C 0.2481(3) 0.04647(14) 1.1101(4) 0.0592(12) Uani 1 1 d .
H11A H 0.2354 0.0279 1.1588 0.071 Uiso 1 1 calc R
H11B H 0.2797 0.0671 1.1504 0.071 Uiso 1 1 calc R
C36 C 0.0775(3) 0.03779(16) 0.4137(5) 0.0729(15) Uani 1 1 d .
H36 H 0.0224 0.0267 0.3816 0.088 Uiso 1 1 calc R
C37 C 0.0950(3) 0.04618(15) 0.5193(5) 0.0694(14) Uani 1 1 d .
H37 H 0.0526 0.0404 0.5586 0.083 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'
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
Cu2 O7 Cu2 102.80(14) 2_656 .
Cu2 O7 Cu1 112.864(17) 2_656 2_656
Cu2 O7 Cu1 112.634(19) . 2_656
Cu2 O7 Cu1 112.634(18) 2_656 .
Cu2 O7 Cu1 112.864(17) . .
Cu1 O7 Cu1 103.39(14) 2_656 .
C1 O1 Cu1 130.34(7) . .
C1 O1 Cu1 130.35(7) . 2_656
Cu1 O1 Cu1 99.31(14) . 2_656
C20 O4 Cu2 130.40(7) . .
C20 O4 Cu2 130.40(7) . 2_656
Cu2 O4 Cu2 99.21(14) . 2_656
C3 C2 C1 120.0(3) . .
C3 C2 C6 116.3(3) . .
C1 C2 C6 123.6(3) . .
O1 C1 C2 121.3(2) . .
O1 C1 C2 121.3(2) . 2_656
C2 C1 C2 117.4(4) . 2_656
N1 C6 C2 128.3(3) . .
C22 C21 C20 119.1(3) . .
C22 C21 C25 117.1(3) . .
C20 C21 C25 123.8(3) . .
N2 C25 C21 128.0(3) . .
O4 C20 C21 120.8(2) . 2_656
O4 C20 C21 120.8(2) . .
C21 C20 C21 118.4(4) 2_656 .
C32 O6 Cu1 119.8(2) . 2_656
C4 C3 C2 122.8(3) . .
C23 C22 C21 123.1(4) . .
C3 C4 C3 117.0(4) 2_656 .
C3 C4 C5 121.5(2) 2_656 .
C3 C4 C5 121.5(2) . .
C22 C23 C22 117.2(5) 2_656 .
C22 C23 C24 121.4(2) 2_656 .
C22 C23 C24 121.4(2) . .
C13 O2 Cu1 127.8(2) . .
C13 O3 Cu2 118.3(2) . 2_656
O3 C13 O2 126.4(3) . .
O3 C13 C14 118.8(3) . .
O2 C13 C14 114.8(3) . .
C15 C14 C19 117.9(4) . .
C15 C14 C13 121.8(3) . .
C19 C14 C13 120.2(3) . .
C14 C19 C18 121.4(4) . .
C14 C15 C16 121.4(4) . .
C17 C18 C19 119.3(5) . .
C18 C17 C16 120.4(4) . .
C17 C16 C15 119.4(4) . .
O7 Cu1 O2 92.76(10) . .
O7 Cu1 O1 78.65(10) . .
O2 Cu1 O1 168.93(10) . .
O7 Cu1 N1 162.08(9) . .
O2 Cu1 N1 95.29(11) . .
O1 Cu1 N1 91.13(10) . .
O7 Cu1 O6 98.84(6) . 2_656
O2 Cu1 O6 98.72(11) . 2_656
O1 Cu1 O6 89.57(7) . 2_656
N1 Cu1 O6 95.73(10) . 2_656
O7 Cu1 Cu1 38.30(7) . 2_656
O2 Cu1 Cu1 130.71(8) . 2_656
O1 Cu1 Cu1 40.34(7) . 2_656
N1 Cu1 Cu1 129.85(8) . 2_656
O6 Cu1 Cu1 95.55(7) 2_656 2_656
O7 Cu2 O5 93.68(11) . .
O7 Cu2 O4 79.00(10) . .
O5 Cu2 O4 172.25(11) . .
O7 Cu2 N2 162.04(9) . .
O5 Cu2 N2 95.33(11) . .
O4 Cu2 N2 91.06(11) . .
O7 Cu2 O3 96.48(7) . 2_656
O5 Cu2 O3 98.27(11) . 2_656
O4 Cu2 O3 85.19(8) . 2_656
N2 Cu2 O3 97.55(10) . 2_656
O7 Cu2 Cu2 38.60(7) . 2_656
O5 Cu2 Cu2 132.23(8) . 2_656
O4 Cu2 Cu2 40.40(7) . 2_656
N2 Cu2 Cu2 129.78(8) . 2_656
O3 Cu2 Cu2 91.22(7) 2_656 2_656
C6 N1 C7 118.2(3) . .
C6 N1 Cu1 123.3(2) . .
C7 N1 Cu1 118.6(2) . .
O6 C32 O5 126.9(3) . .
O6 C32 C33 121.3(3) . .
O5 C32 C33 111.8(3) . .
C32 O5 Cu2 126.9(2) . .
C25 N2 C26 117.9(3) . .
C25 N2 Cu2 124.2(2) . .
C26 N2 Cu2 117.9(2) . .
N2 C26 C31 117.1(3) . .
N2 C26 C27 108.7(3) . .
C31 C26 C27 109.7(3) . .
N1 C7 C12 117.3(3) . .
N1 C7 C8 108.3(3) . .
C12 C7 C8 109.9(3) . .
C38 C33 C34 119.5(3) . .
C38 C33 C32 121.6(3) . .
C34 C33 C32 118.9(3) . .
C11 C12 C7 109.5(3) . .
C33 C34 C35 120.2(4) . .
C7 C8 C9 110.7(4) . .
C26 C31 C30 109.0(3) . .
C29 C28 C27 111.0(4) . .
C26 C27 C28 110.0(3) . .
C10 C9 C8 112.1(4) . .
C29 C30 C31 111.5(4) . .
C11 C10 C9 110.6(4) . .
C33 C38 C37 120.7(4) . .
C36 C35 C34 119.7(5) . .
C30 C29 C28 110.8(4) . .
C10 C11 C12 111.2(4) . .
C35 C36 C37 120.6(4) . .
C36 C37 C38 119.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O7 Cu2 1.9147(19) 2_656
O7 Cu2 1.9147(19) .
O7 Cu1 1.9182(18) 2_656
O7 Cu1 1.9182(18) .
O1 C1 1.301(5) .
O1 Cu1 1.975(2) .
O1 Cu1 1.975(2) 2_656
O4 C20 1.310(5) .
O4 Cu2 1.965(2) .
O4 Cu2 1.965(2) 2_656
C2 C3 1.397(5) .
C2 C1 1.415(4) .
C2 C6 1.466(4) .
C1 C2 1.415(4) 2_656
C6 N1 1.283(4) .
C21 C22 1.399(5) .
C21 C20 1.420(4) .
C21 C25 1.454(5) .
C25 N2 1.283(4) .
C20 C21 1.420(4) 2_656
O6 C32 1.208(4) .
O6 Cu1 2.324(3) 2_656
C3 C4 1.380(4) .
C22 C23 1.380(5) .
C4 C3 1.380(4) 2_656
C4 C5 1.501(7) .
C23 C22 1.380(5) 2_656
C23 C24 1.518(8) .
O2 C13 1.269(4) .
O2 Cu1 1.952(2) .
O3 C13 1.242(4) .
O3 Cu2 2.343(3) 2_656
C13 C14 1.508(5) .
C14 C15 1.371(6) .
C14 C19 1.378(5) .
C19 C18 1.388(6) .
C15 C16 1.383(6) .
C18 C17 1.363(7) .
C17 C16 1.372(7) .
O8 C39 1.394(8) .
Cu1 N1 2.000(3) .
Cu1 O6 2.324(3) 2_656
Cu1 Cu1 3.0106(8) 2_656
Cu2 O5 1.952(2) .
Cu2 N2 1.991(3) .
Cu2 O3 2.343(3) 2_656
Cu2 Cu2 2.9928(8) 2_656
N1 C7 1.486(4) .
C32 O5 1.304(4) .
C32 C33 1.520(4) .
N2 C26 1.488(4) .
C26 C31 1.513(5) .
C26 C27 1.522(5) .
C7 C12 1.520(5) .
C7 C8 1.522(5) .
C33 C38 1.372(5) .
C33 C34 1.380(6) .
C12 C11 1.518(5) .
C34 C35 1.390(6) .
C8 C9 1.540(6) .
C31 C30 1.532(5) .
C28 C29 1.504(6) .
C28 C27 1.534(6) .
C9 C10 1.518(7) .
C30 C29 1.501(7) .
C10 C11 1.506(7) .
C38 C37 1.385(6) .
C35 C36 1.366(7) .
C36 C37 1.383(8) .
