#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:59:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180459 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/28/7212884.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_7212884
loop_
_publ_author_name
'Fainerman-Melnikova, Marina'
'Clegg, Jack K.'
'Pakchung, Amalie A. H.'
'Jensen, Paul'
'Codd, Rachel'
_publ_section_title
;
 Structural diversity of complexes between Cu(ii) or Ni(ii) and endocyclic
 oxygen- or nitrogen-containing ligands: synthesis, X-ray structure
 determinations and circular dichroism spectra
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4217
_journal_paper_doi               10.1039/c0ce00323a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         '2(C21 H18 Cu2 O17), 8(H2 O)'
_chemical_formula_sum            'C42 H52 Cu4 O42'
_chemical_formula_weight         1483.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 99.318(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.458(2)
_cell_length_b                   15.890(2)
_cell_length_c                   11.4300(10)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.43
_cell_volume                     2770.5(6)
_computing_cell_refinement       'SAINT (Bruker-Nonius, 2003)'
_computing_data_collection       'APEX (Bruker-Nonius, 2003)'
_computing_data_reduction
'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)'
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       ω+φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39772
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.95274
_exptl_absorpt_correction_T_min  0.7590
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'APEX (Bruker-Nonius, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4043
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0281
_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)+(0.0307P)²+6.5393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                3720
_reflns_number_total             4043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00323a.txt
_cod_data_source_block           rc07pj2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7212884
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
C1 C 0.30916(10) 0.23718(10) 0.30618(13) 0.0131(3) Uani 1 1 d . . .
C2 C 0.34416(10) 0.23552(11) 0.19141(14) 0.0139(3) Uani 1 1 d . . .
C3 C 0.33016(11) 0.16985(11) 0.00619(14) 0.0148(3) Uani 1 1 d . . .
C4 C 0.38413(12) 0.22420(12) -0.03324(15) 0.0188(3) Uani 1 1 d . . .
H4 H 0.3936 0.2198 -0.1131 0.023 Uiso 1 1 calc R . .
C5 C 0.43048(12) 0.29207(13) 0.04343(16) 0.0209(3) Uani 1 1 d . . .
H5A H 0.4192 0.3473 0.0037 0.025 Uiso 1 1 calc R . .
H5B H 0.4945 0.2817 0.0560 0.025 Uiso 1 1 calc R . .
C6 C 0.39858(11) 0.29342(12) 0.16077(15) 0.0171(3) Uani 1 1 d . . .
H6 H 0.4180 0.3373 0.2152 0.021 Uiso 1 1 calc R . .
C7 C 0.28045(11) 0.10314(11) -0.06666(14) 0.0153(3) Uani 1 1 d . . .
C8 C 0.37021(10) 0.15669(10) 0.60574(13) 0.0116(3) Uani 1 1 d . . .
C9 C 0.43820(10) 0.10146(10) 0.67600(13) 0.0126(3) Uani 1 1 d . . .
C10 C 0.43606(12) 0.01821(11) 0.67108(17) 0.0205(3) Uani 1 1 d . . .
H10 H 0.3922 -0.0081 0.6152 0.025 Uiso 1 1 calc R . .
C11 C 0.5000 -0.03628(17) 0.7500 0.0327(7) Uani 1 2 d S . .
H11A H 0.4682 -0.0728 0.7989 0.039 Uiso 0.50 1 calc PR . .
H11B H 0.5318 -0.0728 0.7011 0.039 Uiso 0.50 1 calc PR . .
O1 O 0.25434(8) 0.18099(8) 0.32273(11) 0.0171(2) Uani 1 1 d . . .
O2 O 0.33680(8) 0.29507(8) 0.37746(10) 0.0170(2) Uani 1 1 d . . .
O3 O 0.31128(9) 0.16848(8) 0.12077(10) 0.0172(2) Uani 1 1 d . . .
O4 O 0.22958(9) 0.05636(8) -0.02663(11) 0.0194(2) Uani 1 1 d . . .
O5 O 0.29635(9) 0.09999(9) -0.17568(11) 0.0225(3) Uani 1 1 d D . .
H1O H 0.2656(14) 0.0606(11) -0.209(2) 0.027 Uiso 1 1 d D . .
O6 O 0.30313(7) 0.12036(8) 0.55062(11) 0.0157(2) Uani 1 1 d . . .
O7 O 0.38470(8) 0.23472(8) 0.60903(11) 0.0159(2) Uani 1 1 d . . .
O8 O 0.5000 0.14811(10) 0.7500 0.0144(3) Uani 1 2 d S . .
O9 O 0.11714(8) 0.07755(8) 0.42600(12) 0.0208(3) Uani 1 1 d D . .
H2O H 0.0905(15) 0.0746(17) 0.4873(14) 0.031 Uiso 1 1 d D . .
H3O H 0.1482(14) 0.0320(9) 0.425(2) 0.031 Uiso 1 1 d D . .
O10 O 0.21409(9) 0.02506(9) 0.21087(11) 0.0215(3) Uani 1 1 d D . .
H4O H 0.2217(17) 0.0282(17) 0.1372(7) 0.032 Uiso 1 1 d D . .
H5O H 0.2268(17) 0.0736(8) 0.244(2) 0.032 Uiso 1 1 d D . .
O11 O 0.0000 0.1433(3) 0.2500 0.0265(8) Uiso 0.50 2 d SPD A 1
H6O H 0.037(3) 0.1235(11) 0.207(5) 0.040 Uiso 0.25 1 d PD B 1
H7O H 0.0000 0.1981(3) 0.2500 0.040 Uiso 0.50 2 d SPD C 1
O11A O 0.0261(4) 0.1459(4) 0.2202(6) 0.0265(8) Uiso 0.25 1 d PD . 2
H6O1 H -0.016(5) 0.115(6) 0.183(9) 0.040 Uiso 0.25 1 d PD D 2
H7O1 H 0.0000 0.1874(6) 0.2500 0.040 Uiso 0.50 2 d SPD E 2
O12 O 0.0417(2) 0.0324(2) 0.6249(4) 0.0429(9) Uani 0.50 1 d PD . .
H8O H 0.013(4) -0.010(3) 0.591(6) 0.064 Uiso 0.50 1 d PD . .
H9O H 0.085(3) 0.015(4) 0.677(5) 0.064 Uiso 0.50 1 d PD . .
Cu1 Cu 0.201724(12) 0.183680(12) 0.469601(15) 0.01009(6) 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'
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 C1 O1 125.79(15) . .
O2 C1 C2 116.58(14) . .
O1 C1 C2 117.63(14) . .
C6 C2 O3 124.54(15) . .
C6 C2 C1 123.47(15) . .
O3 C2 C1 111.97(14) . .
C4 C3 O3 124.73(15) . .
C4 C3 C7 124.79(15) . .
O3 C3 C7 110.48(14) . .
C3 C4 C5 122.47(15) . .
C3 C4 H4 118.8 . .
C5 C4 H4 118.8 . .
C4 C5 C6 109.73(15) . .
C4 C5 H5A 109.7 . .
C6 C5 H5A 109.7 . .
C4 C5 H5B 109.7 . .
C6 C5 H5B 109.7 . .
H5A C5 H5B 108.2 . .
C2 C6 C5 122.54(16) . .
C2 C6 H6 118.7 . .
C5 C6 H6 118.7 . .
O4 C7 O5 124.31(16) . .
O4 C7 C3 122.01(14) . .
O5 C7 C3 113.68(15) . .
O7 C8 O6 126.36(15) . .
O7 C8 C9 117.05(13) . .
O6 C8 C9 116.59(14) . .
C10 C9 O8 124.82(15) . .
C10 C9 C8 123.49(14) . .
O8 C9 C8 111.62(14) . .
C9 C10 C11 122.78(17) . .
C9 C10 H10 118.6 . .
C11 C10 H10 118.6 . .
C10 C11 C10 109.5(2) 2_656 .
C10 C11 H11A 109.8 2_656 .
C10 C11 H11A 109.8 . .
C10 C11 H11B 109.8 2_656 .
C10 C11 H11B 109.8 . .
H11A C11 H11B 108.2 . .
C1 O1 Cu1 119.21(11) . .
C1 O2 Cu1 125.60(11) . 7_556
C2 O3 C3 115.19(13) . .
C7 O5 H1O 106.4(18) . .
C8 O6 Cu1 121.97(11) . .
C8 O7 Cu1 122.00(10) . 7_556
C9 O8 C9 115.24(18) . 2_656
Cu1 O9 H2O 101.9(18) . .
Cu1 O9 H3O 110.0(17) . .
H2O O9 H3O 108(2) . .
H4O O10 H5O 109(2) . .
H6O O11 H7O 111.2(12) . .
H6O O11 H6O1 56(7) . .
H7O O11 H6O1 120(7) . .
H6O O11 H7O1 111.2(12) . .
H6O1 O11 H7O1 120(7) . .
O11A O11A H6O 124(2) 2 .
O11A O11A H7O 55.5(4) 2 .
H6O O11A H7O 180(9) . .
O11A O11A H6O1 76(8) 2 .
H6O O11A H6O1 71(10) . .
H7O O11A H6O1 109(8) . .
O11A O11A H7O1 49.2(6) 2 .
H6O O11A H7O1 173(3) . .
H6O1 O11A H7O1 105(8) . .
H8O O12 H9O 111(7) . .
O6 Cu1 O2 90.13(5) . 7_556
O6 Cu1 O7 169.22(5) . 7_556
O2 Cu1 O7 90.68(5) 7_556 7_556
O6 Cu1 O1 89.01(5) . .
O2 Cu1 O1 169.35(5) 7_556 .
O7 Cu1 O1 88.21(5) 7_556 .
O6 Cu1 O9 96.71(5) . .
O2 Cu1 O9 94.63(5) 7_556 .
O7 Cu1 O9 93.94(5) 7_556 .
O1 Cu1 O9 96.02(5) . .
O6 Cu1 Cu1 84.83(4) . 7_556
O2 Cu1 Cu1 82.36(4) 7_556 7_556
O7 Cu1 Cu1 84.63(4) 7_556 7_556
O1 Cu1 Cu1 86.99(4) . 7_556
O9 Cu1 Cu1 176.64(4) . 7_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.257(2) .
C1 O1 1.266(2) .
C1 C2 1.498(2) .
C2 C6 1.331(2) .
C2 O3 1.383(2) .
C3 C4 1.329(2) .
C3 O3 1.3873(19) .
C3 C7 1.483(2) .
C4 C5 1.497(3) .
C4 H4 0.9500 .
C5 C6 1.502(2) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6 0.9500 .
C7 O4 1.223(2) .
C7 O5 1.3095(19) .
C8 O7 1.259(2) .
C8 O6 1.2625(19) .
C8 C9 1.499(2) .
C9 C10 1.324(2) .
C9 O8 1.3842(17) .
C10 C11 1.501(2) .
C10 H10 0.9500 .
C11 C10 1.501(2) 2_656
C11 H11A 0.9900 .
C11 H11B 0.9900 .
O1 Cu1 1.9808(12) .
O2 Cu1 1.9651(12) 7_556
O5 H1O 0.839(19) .
O6 Cu1 1.9639(12) .
O7 Cu1 1.9711(12) 7_556
O8 C9 1.3842(17) 2_656
O9 Cu1 2.1426(13) .
O9 H2O 0.870(17) .
O9 H3O 0.870(11) .
O10 H4O 0.870(11) .
O10 H5O 0.868(16) .
O11 H6O 0.870(1) .
O11 H7O 0.870(1) .
O11 H6O1 0.89(7) .
O11 H7O1 0.700(11) .
O11A O11A 1.138(13) 2
O11A H6O 0.431(13) .
O11A H7O 1.005(9) .
O11A H6O1 0.870(1) .
O11A H7O1 0.870(1) .
O12 H8O 0.8698(10) .
O12 H9O 0.8698(10) .
Cu1 O2 1.9651(12) 7_556
Cu1 O7 1.9711(12) 7_556
Cu1 Cu1 2.6109(4) 7_556
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H1O O10 0.839(19) 1.76(2) 2.5909(19) 172(3) 6
O9 H2O O12 0.870(19) 1.968(9) 2.811(4) 163(3) .
O9 H3O O4 0.870(13) 1.907(9) 2.7454(18) 161(3) 6_556
O10 H4O O4 0.870(13) 1.949(6) 2.8079(17) 169(3) .
O10 H5O O1 0.868(16) 1.944(16) 2.8113(19) 179(3) .
O10 H5O O3 0.868(16) 2.56(2) 3.0021(19) 112(2) .
O11 H7O O7 0.870(1) 2.446(2) 2.932(3) 115.88(11) 7_556
O11 H7O O7 0.870(1) 2.446(2) 2.932(3) 115.88(11) 8_455
O11 H7O O8 0.870(1) 2.444(5) 3.314(5) 180.000(1) 7_556
O11A H6O1 O9 0.870(1) 1.93(3) 2.771(6) 163(11) 2
O11A H6O1 O12 0.870(1) 2.63(11) 3.059(7) 112(9) 6
O11A H7O1 O7 0.870(1) 2.525(4) 3.015(6) 116.4(4) 8_455
O11A H7O1 O8 0.870(1) 2.614(9) 3.322(7) 139.2(6) 7_556
O12 H8O O9 0.8698(10) 2.25(4) 2.993(4) 143(6) 5_556
O12 H8O O12 0.8698(10) 2.50(6) 3.111(10) 128(6) 5_556
O12 H9O O10 0.8698(10) 2.07(4) 2.838(4) 147(6) 6_556
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_4
O2 C1 C2 C6 -3.1(2) .
O1 C1 C2 C6 176.48(16) .
O2 C1 C2 O3 178.61(14) .
O1 C1 C2 O3 -1.8(2) .
O3 C3 C4 C5 -0.8(3) .
C7 C3 C4 C5 178.02(16) .
C3 C4 C5 C6 -6.2(3) .
O3 C2 C6 C5 0.2(3) .
C1 C2 C6 C5 -177.90(16) .
C4 C5 C6 C2 6.5(2) .
C4 C3 C7 O4 -177.77(17) .
O3 C3 C7 O4 1.2(2) .
C4 C3 C7 O5 2.1(3) .
O3 C3 C7 O5 -178.93(14) .
O7 C8 C9 C10 -172.80(17) .
O6 C8 C9 C10 8.4(2) .
O7 C8 C9 O8 10.24(19) .
O6 C8 C9 O8 -168.54(12) .
O8 C9 C10 C11 2.2(3) .
C8 C9 C10 C11 -174.32(13) .
C9 C10 C11 C10 -1.07(13) 2_656
O2 C1 O1 Cu1 2.5(2) .
C2 C1 O1 Cu1 -177.05(10) .
O1 C1 O2 Cu1 -2.8(2) 7_556
C2 C1 O2 Cu1 176.76(10) 7_556
C6 C2 O3 C3 -7.6(2) .
C1 C2 O3 C3 170.70(13) .
C4 C3 O3 C2 7.9(2) .
C7 C3 O3 C2 -171.06(14) .
O7 C8 O6 Cu1 -5.9(2) .
C9 C8 O6 Cu1 172.75(10) .
O6 C8 O7 Cu1 2.8(2) 7_556
C9 C8 O7 Cu1 -175.80(10) 7_556
C10 C9 O8 C9 -1.14(14) 2_656
C8 C9 O8 C9 175.77(15) 2_656
C8 O6 Cu1 O2 -77.69(12) 7_556
C8 O6 Cu1 O7 16.6(3) 7_556
C8 O6 Cu1 O1 91.70(12) .
C8 O6 Cu1 O9 -172.36(12) .
C8 O6 Cu1 Cu1 4.63(12) 7_556
C1 O1 Cu1 O6 -85.90(13) .
C1 O1 Cu1 O2 -0.5(4) 7_556
C1 O1 Cu1 O7 83.68(13) 7_556
C1 O1 Cu1 O9 177.45(12) .
C1 O1 Cu1 Cu1 -1.03(12) 7_556
