#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:37:28 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702695.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_7702695
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                 109.934(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.126(3)
_cell_length_b                   13.809(3)
_cell_length_c                   15.151(3)
_cell_measurement_reflns_used    976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.93
_cell_volume                     3368.4(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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22274
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.94
_diffrn_standards_interval_count 'end of measurement'
_diffrn_standards_number         '100 first frames'
_exptl_absorpt_coefficient_mu    1.945
_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    1.730
_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         0.938
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0532P)²+4.5112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                3737
_reflns_number_total             5122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106983g.txt
_cod_data_source_block           C36_H38_Cu3_N4_O10_at_100_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        3368.4(11)
_cod_original_sg_symbol_H-M      'C2/c (No.15)'
_cod_database_code               7702695
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu2 Cu 0.5000 0.18096(3) 0.2500 0.01906(10) Uani 1 2 d S . .
Cu1 Cu 0.463774(15) -0.02439(2) 0.115356(19) 0.01666(9) Uani 1 1 d . . .
N16 N 0.40846(12) -0.14986(14) 0.10250(13) 0.0185(4) Uani 1 1 d . . .
O10 O 0.36793(9) 0.04922(11) 0.10733(11) 0.0179(3) Uani 1 1 d . . .
O11 O 0.24628(10) 0.17858(12) 0.07383(13) 0.0224(4) Uani 1 1 d . . .
H11 H 0.2012(18) 0.214(2) 0.049(2) 0.023(7) Uiso 1 1 d . . .
N26 N 0.59115(12) 0.26872(15) 0.26302(16) 0.0266(5) Uani 1 1 d . A .
O20 O 0.53242(9) 0.08698(12) 0.17647(11) 0.0184(3) Uani 1 1 d . . .
O21 O 0.56297(10) -0.06796(13) 0.09558(12) 0.0225(4) Uani 1 1 d . . .
C10 C 0.29226(13) 0.01572(16) 0.09139(15) 0.0159(4) Uani 1 1 d . . .
C11 C 0.22582(13) 0.08319(17) 0.07543(15) 0.0176(4) Uani 1 1 d . . .
C12 C 0.14579(14) 0.05229(18) 0.06157(16) 0.0209(5) Uani 1 1 d . . .
H12 H 0.1030 0.0988 0.0534 0.025 Uiso 1 1 calc R . .
C13 C 0.12680(14) -0.04658(18) 0.05938(17) 0.0230(5) Uani 1 1 d . . .
H13 H 0.0715 -0.0670 0.0498 0.028 Uiso 1 1 calc R . .
C14 C 0.18837(14) -0.11318(17) 0.07117(16) 0.0200(5) Uani 1 1 d . . .
H14 H 0.1755 -0.1802 0.0691 0.024 Uiso 1 1 calc R . .
C15 C 0.27165(13) -0.08370(17) 0.08657(15) 0.0174(4) Uani 1 1 d . . .
C16 C 0.33088(14) -0.15892(17) 0.09229(15) 0.0183(4) Uani 1 1 d . . .
H16 H 0.3105 -0.2234 0.0880 0.022 Uiso 1 1 calc R . .
C17 C 0.45707(14) -0.24002(18) 0.11271(17) 0.0226(5) Uani 1 1 d . . .
H17A H 0.4867 -0.2402 0.0669 0.027 Uiso 1 1 calc R . .
H17B H 0.4191 -0.2964 0.0992 0.027 Uiso 1 1 calc R . .
C18 C 0.51985(14) -0.24861(17) 0.21203(17) 0.0216(5) Uani 1 1 d . . .
H18A H 0.5595 -0.1939 0.2235 0.026 Uiso 1 1 calc R . .
H18B H 0.5518 -0.3093 0.2168 0.026 Uiso 1 1 calc R . .
C20 C 0.60812(13) 0.08245(18) 0.16894(16) 0.0190(4) Uani 1 1 d . . .
C21 C 0.62457(14) -0.00234(18) 0.12657(16) 0.0202(5) Uani 1 1 d . . .
C22 C 0.70243(14) -0.0134(2) 0.11838(17) 0.0242(5) Uani 1 1 d . . .
H22 H 0.7147 -0.0704 0.0906 0.029 Uiso 1 1 calc R . .
C23 C 0.76292(15) 0.0586(2) 0.15058(19) 0.0284(6) Uani 1 1 d . . .
H23 H 0.8158 0.0502 0.1441 0.034 Uiso 1 1 calc R . .
C24 C 0.74678(14) 0.1404(2) 0.19109(19) 0.0277(6) Uani 1 1 d . . .
H24 H 0.7887 0.1885 0.2131 0.033 Uiso 1 1 calc R . .
C25 C 0.66838(14) 0.15512(18) 0.20091(18) 0.0224(5) Uani 1 1 d . . .
C26 C 0.65599(14) 0.24348(18) 0.24474(19) 0.0277(6) Uani 1 1 d . . .
H26 H 0.7009 0.2881 0.2621 0.033 Uiso 1 1 calc R . .
C27 C 0.5943(2) 0.3627(2) 0.3107(3) 0.0613(13) Uani 1 1 d . . .
H27A H 0.5764 0.3529 0.3656 0.074 Uiso 0.531(7) 1 calc PR A 1
H27B H 0.6526 0.3855 0.3343 0.074 Uiso 0.531(7) 1 calc PR A 1
H27C H 0.6392 0.3564 0.3722 0.074 Uiso 0.469(7) 1 calc PR A 2
H27D H 0.6144 0.4101 0.2742 0.074 Uiso 0.469(7) 1 calc PR A 2
C28 C 0.5427(3) 0.4382(3) 0.2512(3) 0.0229(12) Uani 0.531(7) 1 d P . 1
H28A H 0.5775 0.4755 0.2229 0.027 Uiso 0.531(7) 1 calc PR A 1
H28B H 0.5251 0.4831 0.2918 0.027 Uiso 0.531(7) 1 calc PR A 1
C28' C 0.5345(3) 0.4042(4) 0.3274(3) 0.0196(13) Uani 0.469(7) 1 d P . 2
H28C H 0.5580 0.4616 0.3667 0.023 Uiso 0.469(7) 1 calc PR A 2
H28D H 0.5156 0.3594 0.3670 0.023 Uiso 0.469(7) 1 calc PR A 2
O1W O 0.10958(11) 0.28690(14) -0.00198(14) 0.0249(4) Uani 1 1 d . . .
H1W H 0.094(2) 0.325(2) 0.029(2) 0.034(9) Uiso 1 1 d . . .
H2W H 0.127(3) 0.320(3) -0.042(3) 0.074(15) 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 161.70(7) . .
O10 Cu1 N16 95.12(7) . .
O21 Cu1 N16 97.55(8) . .
O10 Cu1 O20 88.65(7) . .
O21 Cu1 O20 84.25(7) . .
N16 Cu1 O20 158.98(8) . .
O20 Cu2 O20 94.50(10) . 2_655
O20 Cu2 N26 95.75(8) . .
O20 Cu2 N26 138.69(8) 2_655 .
O20 Cu2 N26 138.69(8) . 2_655
O20 Cu2 N26 95.75(8) 2_655 2_655
N26 Cu2 N26 102.32(12) . 2_655
C16 N16 C17 116.8(2) . .
C16 N16 Cu1 122.88(16) . .
C17 N16 Cu1 120.06(15) . .
C10 O10 Cu1 126.73(15) . .
C26 N26 C27 117.0(3) . .
C26 N26 Cu2 122.47(17) . .
C27 N26 Cu2 119.7(2) . .
C20 O20 Cu2 124.23(15) . .
C20 O20 Cu1 111.33(15) . .
Cu2 O20 Cu1 124.04(8) . .
C21 O21 Cu1 111.36(15) . .
O10 C10 C15 124.3(2) . .
O10 C10 C11 118.6(2) . .
C15 C10 C11 117.08(19) . .
O11 C11 C12 122.9(2) . .
O11 C11 C10 116.02(19) . .
C12 C11 C10 121.1(2) . .
C11 C12 C13 121.0(2) . .
C14 C13 C12 119.4(2) . .
C13 C14 C15 121.0(2) . .
C10 C15 C14 120.3(2) . .
C10 C15 C16 122.8(2) . .
C14 C15 C16 116.8(2) . .
N16 C16 C15 128.0(2) . .
N16 C17 C18 110.57(19) . .
C17 C18 C18 113.5(2) . 2_655
O20 C20 C25 123.8(2) . .
O20 C20 C21 115.3(2) . .
C25 C20 C21 120.9(2) . .
O21 C21 C22 123.8(2) . .
O21 C21 C20 117.6(2) . .
C22 C21 C20 118.6(2) . .
C21 C22 C23 120.7(3) . .
C24 C23 C22 120.6(2) . .
C23 C24 C25 120.9(2) . .
C20 C25 C24 118.3(2) . .
C20 C25 C26 124.0(2) . .
C24 C25 C26 117.7(2) . .
N26 C26 C25 127.3(2) . .
C28' C27 C28 56.2(3) . .
C28' C27 N26 126.5(4) . .
C28 C27 N26 114.3(3) . .
C27 C28 C28' 116.4(4) . 2_655
C27 C28' C28 121.7(4) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O10 1.8989(16) .
Cu1 O21 1.9195(16) .
Cu1 N16 1.952(2) .
Cu1 O20 1.9653(16) .
Cu1 Cu1 3.8385(9) 2_655
Cu1 Cu2 3.4241(6) .
Cu2 O20 1.9119(17) .
Cu2 O20 1.9119(17) 2_655
Cu2 N26 1.933(2) .
Cu2 N26 1.933(2) 2_655
N16 C16 1.290(3) .
N16 C17 1.476(3) .
N16 N16 4.500(4) 2_655
O10 C10 1.319(3) .
O10 O10 5.081(3) 2_655
O11 C11 1.365(3) .
O11 O11 8.508(4) 2_655
N26 C26 1.281(3) .
N26 C27 1.477(4) .
N26 N26 3.011(4) 2_655
O20 C20 1.341(3) .
O20 O20 2.808(3) 2_655
O21 C21 1.348(3) .
O21 O21 5.782(3) 2_655
C10 C15 1.413(3) .
C10 C11 1.426(3) .
C11 C12 1.381(3) .
C12 C13 1.401(3) .
C13 C14 1.364(3) .
C14 C15 1.424(3) .
C15 C16 1.434(3) .
C17 C18 1.527(3) .
C18 C18 1.523(5) 2_655
C20 C25 1.402(3) .
C20 C21 1.409(4) .
C21 C22 1.389(3) .
C22 C23 1.398(4) .
C23 C24 1.359(4) .
C24 C25 1.415(3) .
C25 C26 1.439(4) .
C27 C28' 1.273(6) .
C27 C28 1.461(5) .
C28 C28' 1.521(6) 2_655
C28' C28 1.521(6) 2_655
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
O10 Cu1 N16 C16 0.27(19) . . .
O21 Cu1 N16 C16 -166.49(18) . . .
O20 Cu1 N16 C16 99.9(3) . . .
O10 Cu1 N16 C17 -174.24(17) . . .
O21 Cu1 N16 C17 19.00(18) . . .
O20 Cu1 N16 C17 -74.6(3) . . .
O21 Cu1 O10 C10 129.6(2) . . .
N16 Cu1 O10 C10 -4.08(18) . . .
O20 Cu1 O10 C10 -163.36(18) . . .
O20 Cu2 N26 C26 -15.3(2) . . .
O20 Cu2 N26 C26 88.3(2) 2_655 . .
N26 Cu2 N26 C26 -157.9(3) 2_655 . .
O20 Cu2 N26 C27 175.5(2) . . .
O20 Cu2 N26 C27 -81.0(2) 2_655 . .
N26 Cu2 N26 C27 32.88(18) 2_655 . .
O20 Cu2 O20 C20 -123.51(19) 2_655 . .
N26 Cu2 O20 C20 16.42(18) . . .
N26 Cu2 O20 C20 132.49(18) 2_655 . .
O20 Cu2 O20 Cu1 48.58(7) 2_655 . .
N26 Cu2 O20 Cu1 -171.49(10) . . .
N26 Cu2 O20 Cu1 -55.41(17) 2_655 . .
O10 Cu1 O20 C20 -158.70(15) . . .
O21 Cu1 O20 C20 4.41(14) . . .
N16 Cu1 O20 C20 100.5(2) . . .
O10 Cu1 O20 Cu2 28.32(10) . . .
O21 Cu1 O20 Cu2 -168.57(11) . . .
N16 Cu1 O20 Cu2 -72.5(2) . . .
O10 Cu1 O21 C21 64.4(3) . . .
N16 Cu1 O21 C21 -162.20(15) . . .
O20 Cu1 O21 C21 -3.29(15) . . .
Cu1 O10 C10 C15 6.5(3) . . .
Cu1 O10 C10 C11 -171.79(15) . . .
O10 C10 C11 O11 2.9(3) . . .
C15 C10 C11 O11 -175.52(19) . . .
O10 C10 C11 C12 -177.8(2) . . .
C15 C10 C11 C12 3.8(3) . . .
O11 C11 C12 C13 177.0(2) . . .
C10 C11 C12 C13 -2.3(4) . . .
C11 C12 C13 C14 0.0(4) . . .
C12 C13 C14 C15 0.6(4) . . .
O10 C10 C15 C14 178.5(2) . . .
C11 C10 C15 C14 -3.1(3) . . .
O10 C10 C15 C16 -4.4(3) . . .
C11 C10 C15 C16 173.9(2) . . .
C13 C14 C15 C10 1.0(3) . . .
C13 C14 C15 C16 -176.2(2) . . .
C17 N16 C16 C15 176.0(2) . . .
Cu1 N16 C16 C15 1.3(3) . . .
C10 C15 C16 N16 0.2(4) . . .
C14 C15 C16 N16 177.4(2) . . .
C16 N16 C17 C18 -111.2(2) . . .
Cu1 N16 C17 C18 63.6(2) . . .
N16 C17 C18 C18 59.0(2) . . 2_655
Cu2 O20 C20 C25 -11.1(3) . . .
Cu1 O20 C20 C25 175.92(18) . . .
Cu2 O20 C20 C21 168.33(15) . . .
Cu1 O20 C20 C21 -4.6(2) . . .
Cu1 O21 C21 C22 -177.77(19) . . .
Cu1 O21 C21 C20 1.7(3) . . .
O20 C20 C21 O21 2.1(3) . . .
C25 C20 C21 O21 -178.5(2) . . .
O20 C20 C21 C22 -178.4(2) . . .
C25 C20 C21 C22 1.0(3) . . .
O21 C21 C22 C23 178.8(2) . . .
C20 C21 C22 C23 -0.7(4) . . .
C21 C22 C23 C24 0.4(4) . . .
C22 C23 C24 C25 -0.5(4) . . .
O20 C20 C25 C24 178.3(2) . . .
C21 C20 C25 C24 -1.1(3) . . .
O20 C20 C25 C26 -0.6(4) . . .
C21 C20 C25 C26 180.0(2) . . .
C23 C24 C25 C20 0.8(4) . . .
C23 C24 C25 C26 179.8(2) . . .
C27 N26 C26 C25 178.6(3) . . .
Cu2 N26 C26 C25 9.1(4) . . .
C20 C25 C26 N26 1.6(4) . . .
C24 C25 C26 N26 -177.4(3) . . .
C26 N26 C27 C28' 173.5(4) . . .
Cu2 N26 C27 C28' -16.7(5) . . .
C26 N26 C27 C28 108.7(4) . . .
Cu2 N26 C27 C28 -81.5(4) . . .
C28' C27 C28 C28' -89.9(5) . . 2_655
N26 C27 C28 C28' 29.0(6) . . 2_655
C28 C27 C28' C28 33.2(4) . . 2_655
N26 C27 C28' C28 -63.7(7) . . 2_655
C17 C18 C18 C17 -170.3(3) . 2_655 2_655
C27 C28 C28' C27 65.2(7) . 2_655 2_655
N16 C17 C18 C18 59.0(2) . . 2_655
N26 C27 C28 C28' 29.0(6) . . 2_655
N26 C27 C28' C28 -63.7(7) . . 2_655
