#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:37:28 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702696.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_7702696
loop_
_publ_author_name
'Sanmartín, Jesús'
'Bermejo, Manuel R.'
'García-Deibe, Ana M.'
'Nascimento, Otaciro R.'
'Lezama, Luis'
'Rojo, Teófilo'
_publ_section_title
;
 Magnetic properties of a bishelical [4 + 4 + 4] trinuclear copper(ii)
 complex
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1030
_journal_paper_doi               10.1039/b106983g
_journal_year                    2002
_chemical_formula_sum            'C36 H38 Cu3 N4 O10'
_chemical_formula_weight         877.32
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 110.026(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.171(3)
_cell_length_b                   13.918(3)
_cell_length_c                   15.373(3)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.93
_cell_volume                     3451.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_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  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22891
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.93
_diffrn_standards_interval_count 'end of measurement'
_diffrn_standards_number         '100 first frames'
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.782715
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0570P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                2968
_reflns_number_total             5268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106983g.txt
_cod_data_source_block           C36_H38_Cu3_N4_O10_at_293_K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3451.6(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7702696
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
Cu1 Cu -0.036275(19) -0.02385(3) 0.11635(3) 0.03503(12) Uani 1 1 d .
Cu2 Cu 0.0000 0.17942(3) 0.2500 0.03664(15) Uani 1 2 d S
O10 O -0.13210(11) 0.04902(14) 0.10700(14) 0.0356(5) Uani 1 1 d .
O11 O -0.25330(13) 0.17725(16) 0.07345(17) 0.0456(5) Uani 1 1 d .
H11 H -0.298(2) 0.210(3) 0.050(2) 0.055(11) Uiso 1 1 d .
O20 O 0.03200(10) 0.08665(14) 0.17678(14) 0.0349(4) Uani 1 1 d .
O21 O 0.06295(12) -0.06683(16) 0.09735(15) 0.0438(5) Uani 1 1 d .
N16 N -0.09158(14) -0.14848(17) 0.10388(17) 0.0374(6) Uani 1 1 d .
N26 N 0.09095(14) 0.26676(17) 0.26272(18) 0.0417(6) Uani 1 1 d .
C10 C -0.20770(16) 0.0159(2) 0.09068(18) 0.0310(6) Uani 1 1 d .
C11 C -0.27388(16) 0.0831(2) 0.07434(19) 0.0342(6) Uani 1 1 d .
C12 C -0.35358(17) 0.0523(2) 0.0597(2) 0.0435(7) Uani 1 1 d .
H12 H -0.3956 0.0973 0.0513 0.052 Uiso 1 1 calc R
C13 C -0.37219(18) -0.0461(3) 0.0574(2) 0.0481(8) Uani 1 1 d .
H13 H -0.4263 -0.0661 0.0472 0.058 Uiso 1 1 calc R
C14 C -0.31126(18) -0.1116(2) 0.0701(2) 0.0406(7) Uani 1 1 d .
H14 H -0.3240 -0.1767 0.0683 0.049 Uiso 1 1 calc R
C15 C -0.22795(16) -0.0830(2) 0.08633(19) 0.0338(6) Uani 1 1 d .
C16 C -0.16885(18) -0.1568(2) 0.09316(19) 0.0374(7) Uani 1 1 d .
H16 H -0.1888 -0.2193 0.0894 0.045 Uiso 1 1 calc R
C17 C -0.04259(18) -0.2378(2) 0.1149(2) 0.0458(8) Uani 1 1 d .
H17A H -0.0132 -0.2379 0.0711 0.055 Uiso 1 1 calc R
H17B H -0.0796 -0.2928 0.1015 0.055 Uiso 1 1 calc R
C18 C 0.01922(18) -0.2463(2) 0.2128(2) 0.0472(8) Uani 1 1 d .
H18A H 0.0505 -0.3053 0.2174 0.057 Uiso 1 1 calc R
H18B H 0.0580 -0.1932 0.2239 0.057 Uiso 1 1 calc R
C20 C 0.10790(16) 0.0823(2) 0.16939(19) 0.0327(6) Uani 1 1 d .
C21 C 0.12390(17) -0.0016(2) 0.1277(2) 0.0364(7) Uani 1 1 d .
C22 C 0.20164(18) -0.0122(3) 0.1195(2) 0.0434(7) Uani 1 1 d .
H22 H 0.2138 -0.0675 0.0927 0.052 Uiso 1 1 calc R
C23 C 0.26131(18) 0.0593(3) 0.1509(2) 0.0508(9) Uani 1 1 d .
H23 H 0.3128 0.0514 0.1444 0.061 Uiso 1 1 calc R
C24 C 0.24560(18) 0.1400(3) 0.1908(2) 0.0481(8) Uani 1 1 d .
H24 H 0.2867 0.1865 0.2121 0.058 Uiso 1 1 calc R
C25 C 0.16765(16) 0.1547(2) 0.2007(2) 0.0375(7) Uani 1 1 d .
C26 C 0.15515(17) 0.2420(2) 0.2438(2) 0.0426(8) Uani 1 1 d .
H26 H 0.1988 0.2856 0.2600 0.051 Uiso 1 1 calc R
C27 C 0.0873(14) 0.3571(12) 0.3195(13) 0.043(3) Uani 0.54(4) 1 d P
H27A H 0.0575 0.3432 0.3615 0.052 Uiso 0.54(4) 1 calc PR
H27B H 0.1428 0.3780 0.3558 0.052 Uiso 0.54(4) 1 calc PR
C27' C 0.1027(14) 0.3654(16) 0.295(2) 0.049(4) Uani 0.46(4) 1 d P
H27C H 0.1062 0.4061 0.2449 0.059 Uiso 0.46(4) 1 calc PR
H27D H 0.1550 0.3704 0.3456 0.059 Uiso 0.46(4) 1 calc PR
C28 C 0.0426(4) 0.4351(4) 0.2511(5) 0.051(2) Uani 0.558(9) 1 d P
H28A H 0.0809 0.4618 0.2236 0.061 Uiso 0.558(9) 1 calc PR
H28B H 0.0273 0.4863 0.2850 0.061 Uiso 0.558(9) 1 calc PR
C28' C 0.0349(4) 0.4016(5) 0.3261(5) 0.043(2) Uani 0.442(9) 1 d P
H28C H 0.0561 0.4547 0.3685 0.051 Uiso 0.442(9) 1 calc PR
H28D H 0.0194 0.3509 0.3603 0.051 Uiso 0.442(9) 1 calc PR
O1W O -0.39001(16) 0.28787(18) -0.0001(2) 0.0529(6) Uani 1 1 d .
H1W H -0.412(2) 0.324(2) 0.027(2) 0.040(10) Uiso 1 1 d .
H2W H -0.374(3) 0.313(4) -0.051(4) 0.14(2) Uiso 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'
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'
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
O10 Cu1 O21 161.33(10) . .
O10 Cu1 N16 95.01(9) . .
O21 Cu1 N16 97.77(10) . .
O10 Cu1 O20 88.79(8) . .
O21 Cu1 O20 84.20(8) . .
N16 Cu1 O20 158.81(10) . .
O20 Cu2 O20 95.10(12) . 2
O20 Cu2 N26 95.68(10) . .
O20 Cu2 N26 138.50(9) 2 .
O20 Cu2 N26 138.50(9) . 2
O20 Cu2 N26 95.68(10) 2 2
N26 Cu2 N26 102.18(15) . 2
C10 O10 Cu1 126.84(18) . .
C20 O20 Cu2 124.11(18) . .
C20 O20 Cu1 111.28(18) . .
Cu2 O20 Cu1 124.17(9) . .
C21 O21 Cu1 111.29(18) . .
C16 N16 C17 117.5(3) . .
C16 N16 Cu1 122.5(2) . .
C17 N16 Cu1 119.78(19) . .
C26 N26 C27' 107.6(11) . .
C26 N26 C27 123.6(9) . .
C27' N26 C27 20.7(7) . .
C26 N26 Cu2 122.4(2) . .
C27' N26 Cu2 130.0(11) . .
C27 N26 Cu2 112.4(9) . .
O10 C10 C15 124.0(2) . .
O10 C10 C11 118.5(3) . .
C15 C10 C11 117.5(2) . .
O11 C11 C12 123.1(3) . .
O11 C11 C10 116.1(2) . .
C12 C11 C10 120.8(3) . .
C11 C12 C13 120.8(3) . .
C14 C13 C12 119.8(3) . .
C13 C14 C15 121.3(3) . .
C10 C15 C16 122.8(2) . .
C10 C15 C14 119.8(3) . .
C16 C15 C14 117.4(3) . .
N16 C16 C15 128.6(3) . .
N16 C17 C18 110.8(2) . .
C18 C18 C17 114.4(3) 2 .
O20 C20 C25 123.7(3) . .
O20 C20 C21 115.0(2) . .
C25 C20 C21 121.4(3) . .
O21 C21 C22 123.7(3) . .
O21 C21 C20 118.0(2) . .
C22 C21 C20 118.3(3) . .
C23 C22 C21 120.5(3) . .
C24 C23 C22 121.0(3) . .
C23 C24 C25 120.9(3) . .
C20 C25 C24 117.9(3) . .
C20 C25 C26 124.1(3) . .
C24 C25 C26 118.0(3) . .
N26 C26 C25 127.6(3) . .
C28 C27 N26 107.4(11) . .
N26 C27' C28' 113.3(17) . .
C27 C28 C28' 114.8(8) . 2
C27' C28' C28 114.9(13) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O10 1.8959(18) .
Cu1 O21 1.9200(19) .
Cu1 N16 1.955(2) .
Cu1 O20 1.9639(19) .
Cu1 Cu1 3.8640(10) 2
Cu1 Cu2 3.4259(7) .
Cu2 O20 1.9130(19) .
Cu2 O20 1.9130(19) 2
Cu2 N26 1.935(2) .
Cu2 N26 1.935(2) 2
O10 C10 1.318(3) .
O10 O10 5.123(4) 2
O11 C11 1.358(4) .
O11 O11 8.532(5) 2
O11 H11 0.85(4) .
O20 C20 1.348(3) .
O20 O20 2.823(4) 2
O21 C21 1.343(4) .
O21 O21 5.801(4) 2
N16 C16 1.285(4) .
N16 C17 1.478(4) .
N16 N16 4.516(5) 2
N26 C26 1.280(4) .
N26 C27' 1.45(2) .
N26 C27 1.545(17) .
N26 N26 3.012(5) 2
C10 C15 1.415(4) .
C10 C11 1.427(4) .
C11 C12 1.377(4) .
C12 C13 1.404(5) .
C13 C14 1.350(4) .
C14 C15 1.422(4) .
C15 C16 1.422(4) .
C17 C18 1.520(4) .
C18 C18 1.505(7) 2
C20 C25 1.401(4) .
C20 C21 1.404(4) .
C21 C22 1.391(4) .
C22 C23 1.390(5) .
C23 C24 1.351(5) .
C24 C25 1.413(4) .
C25 C26 1.434(4) .
C27 C28 1.523(18) .
C27' C28' 1.49(3) .
C28 C28' 1.522(9) 2
C28' C28 1.522(9) 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O21 Cu1 O10 C10 129.0(3) . . .
N16 Cu1 O10 C10 -4.1(2) . . .
O20 Cu1 O10 C10 -163.2(2) . . .
O20 Cu2 O20 C20 -123.1(2) 2 . .
N26 Cu2 O20 C20 16.8(2) . . .
N26 Cu2 O20 C20 132.4(2) 2 . .
O20 Cu2 O20 Cu1 48.56(9) 2 . .
N26 Cu2 O20 Cu1 -171.58(13) . . .
N26 Cu2 O20 Cu1 -56.0(2) 2 . .
O10 Cu1 O20 C20 -158.09(18) . . .
O21 Cu1 O20 C20 4.58(18) . . .
N16 Cu1 O20 C20 101.1(3) . . .
O10 Cu1 O20 Cu2 29.31(13) . . .
O21 Cu1 O20 Cu2 -168.02(14) . . .
N16 Cu1 O20 Cu2 -71.5(3) . . .
O10 Cu1 O21 C21 64.9(3) . . .
N16 Cu1 O21 C21 -162.33(19) . . .
O20 Cu1 O21 C21 -3.58(19) . . .
O10 Cu1 N16 C16 0.3(2) . . .
O21 Cu1 N16 C16 -166.1(2) . . .
O20 Cu1 N16 C16 99.9(3) . . .
O10 Cu1 N16 C17 -174.4(2) . . .
O21 Cu1 N16 C17 19.3(2) . . .
O20 Cu1 N16 C17 -74.7(3) . . .
O20 Cu2 N26 C26 -15.0(3) . . .
O20 Cu2 N26 C26 89.3(3) 2 . .
N26 Cu2 N26 C26 -157.3(3) 2 . .
O20 Cu2 N26 C27' 166.5(16) . . .
O20 Cu2 N26 C27' -89.2(16) 2 . .
N26 Cu2 N26 C27' 24.2(16) 2 . .
O20 Cu2 N26 C27 179.3(7) . . .
O20 Cu2 N26 C27 -76.4(7) 2 . .
N26 Cu2 N26 C27 37.0(7) 2 . .
Cu1 O10 C10 C15 6.5(4) . . .
Cu1 O10 C10 C11 -172.06(19) . . .
O10 C10 C11 O11 2.5(4) . . .
C15 C10 C11 O11 -176.2(3) . . .
O10 C10 C11 C12 -178.0(3) . . .
C15 C10 C11 C12 3.3(4) . . .
O11 C11 C12 C13 177.2(3) . . .
C10 C11 C12 C13 -2.2(5) . . .
C11 C12 C13 C14 0.3(5) . . .
C12 C13 C14 C15 0.3(5) . . .
O10 C10 C15 C16 -4.3(4) . . .
C11 C10 C15 C16 174.3(3) . . .
O10 C10 C15 C14 178.7(3) . . .
C11 C10 C15 C14 -2.7(4) . . .
C13 C14 C15 C10 1.0(4) . . .
C13 C14 C15 C16 -176.1(3) . . .
C17 N16 C16 C15 176.2(3) . . .
Cu1 N16 C16 C15 1.4(4) . . .
C10 C15 C16 N16 0.1(5) . . .
C14 C15 C16 N16 177.1(3) . . .
C16 N16 C17 C18 -110.9(3) . . .
Cu1 N16 C17 C18 64.0(3) . . .
N16 C17 C18 C18 58.8(3) . . 2
Cu2 O20 C20 C25 -11.8(4) . . .
Cu1 O20 C20 C25 175.6(2) . . .
Cu2 O20 C20 C21 167.96(19) . . .
Cu1 O20 C20 C21 -4.7(3) . . .
Cu1 O21 C21 C22 -177.5(2) . . .
Cu1 O21 C21 C20 2.1(3) . . .
O20 C20 C21 O21 1.8(4) . . .
C25 C20 C21 O21 -178.5(3) . . .
O20 C20 C21 C22 -178.6(2) . . .
C25 C20 C21 C22 1.1(4) . . .
O21 C21 C22 C23 178.8(3) . . .
C20 C21 C22 C23 -0.7(5) . . .
C21 C22 C23 C24 0.6(5) . . .
C22 C23 C24 C25 -0.8(5) . . .
O20 C20 C25 C24 178.4(3) . . .
C21 C20 C25 C24 -1.3(4) . . .
O20 C20 C25 C26 -0.3(5) . . .
C21 C20 C25 C26 180.0(3) . . .
C23 C24 C25 C20 1.1(5) . . .
C23 C24 C25 C26 179.9(3) . . .
C27' N26 C26 C25 -172.7(13) . . .
C27 N26 C26 C25 172.6(9) . . .
Cu2 N26 C26 C25 8.5(5) . . .
C20 C25 C26 N26 2.0(5) . . .
C24 C25 C26 N26 -176.7(3) . . .
C26 N26 C27 C28 100.1(12) . . .
C27' N26 C27 C28 57(4) . . .
Cu2 N26 C27 C28 -94.3(13) . . .
C26 N26 C27' C28' -175.7(14) . . .
C27 N26 C27' C28' -32(3) . . .
Cu2 N26 C27' C28' 3(3) . . .
N26 C27 C28 C28' 44.2(17) . . 2
N26 C27' C28' C28 -81(2) . . 2
C17 C18 C18 C17 -170.2(4) . 2 2
C27 C28 C28' C27' 62.8(19) . 2 2
C27' C28' C28 C27 62.8(19) . 2 2
N16 C17 C18 C18 58.8(3) . . 2
N26 C27 C28 C28' 44.2(17) . . 2
N26 C27' C28' C28 -81(2) . . 2
