#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:17:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180421 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209053.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_7209053
loop_
_publ_author_name
'Ion, Adrian E.'
'Nica, Simona'
'Madalan, Augustin M.'
'Lloret, Francesc'
'Julve, Miguel'
'Andruh, Marius'
_publ_section_title
;
 C3-symmetric trinuclear copper(ii) species as tectons in crystal
 engineering
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              294
_journal_paper_doi               10.1039/c2ce26469b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C49 H64 Cu3 N6 O13'
_chemical_formula_weight         1135.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.274(3)
_cell_length_b                   20.274(3)
_cell_length_c                   11.094(2)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      3.48
_cell_volume                     3949.1(11)
_computing_cell_refinement       X-Area
_computing_data_collection       X-Area
_computing_data_reduction        X-Area
_computing_molecular_graphics    'Diamond 3.1, 2006'
_computing_publication_material  'Diamond 3.1, 2006'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega 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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13105
_diffrn_reflns_theta_full        26.21
_diffrn_reflns_theta_max         26.21
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  1.0383
_exptl_absorpt_correction_T_min  0.3156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1773
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3538
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0357P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                3047
_reflns_number_total             3538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26469b.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3949.3(11)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7209053
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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 0.40210(19) 0.66276(19) 0.7253(3) 0.0352(7) Uani 1 1 d . . .
C2 C 0.40587(18) 0.73470(18) 0.7255(3) 0.0361(7) Uani 1 1 d . . .
C3 C 0.4760(2) 0.8043(2) 0.7237(3) 0.0418(8) Uani 1 1 d . A .
H3 H 0.4731 0.8487 0.7200 0.050 Uiso 1 1 calc R . .
C4 C 0.6097(2) 0.8891(2) 0.7179(6) 0.0725(14) Uani 0.80 1 d P A 1
H4A H 0.5997 0.9253 0.7595 0.087 Uiso 0.80 1 calc PR A 1
H4B H 0.6205 0.9043 0.6341 0.087 Uiso 0.80 1 calc PR A 1
C5 C 0.6753(3) 0.8880(3) 0.7735(8) 0.0762(19) Uani 0.80 1 d P A 1
H5A H 0.6710 0.8883 0.8605 0.091 Uiso 0.80 1 calc PR A 1
H5B H 0.7219 0.9335 0.7500 0.091 Uiso 0.80 1 calc PR A 1
C6 C 0.7050(5) 0.8221(6) 0.6170(8) 0.090(3) Uani 0.80 1 d P A 1
H6A H 0.7052 0.7757 0.6003 0.135 Uiso 0.80 1 calc PR A 1
H6B H 0.7557 0.8646 0.6082 0.135 Uiso 0.80 1 calc PR A 1
H6C H 0.6716 0.8274 0.5616 0.135 Uiso 0.80 1 calc PR A 1
C7 C 0.7320(4) 0.8124(5) 0.8232(7) 0.082(2) Uani 0.80 1 d P A 1
H7A H 0.7143 0.8104 0.9041 0.123 Uiso 0.80 1 calc PR A 1
H7B H 0.7824 0.8554 0.8149 0.123 Uiso 0.80 1 calc PR A 1
H7C H 0.7329 0.7664 0.8061 0.123 Uiso 0.80 1 calc PR A 1
C4A C 0.6097(2) 0.8891(2) 0.7179(6) 0.0725(14) Uani 0.20 1 d P A 2
H4A1 H 0.5983 0.9208 0.6665 0.087 Uiso 0.20 1 calc PR A 2
H4A2 H 0.6236 0.9124 0.7971 0.087 Uiso 0.20 1 calc PR A 2
C5A C 0.6707(9) 0.8819(9) 0.6680(17) 0.036(4) Uani 0.20 1 d P A 2
H5A1 H 0.7177 0.9303 0.6736 0.043 Uiso 0.20 1 calc PR A 2
H5A2 H 0.6606 0.8682 0.5835 0.043 Uiso 0.20 1 calc PR A 2
C6A C 0.7292(19) 0.798(3) 0.654(4) 0.13(2) Uani 0.20 1 d P A 2
H6A1 H 0.7044 0.7804 0.5773 0.189 Uiso 0.20 1 calc PR A 2
H6A2 H 0.7348 0.7589 0.6921 0.189 Uiso 0.20 1 calc PR A 2
H6A3 H 0.7785 0.8423 0.6418 0.189 Uiso 0.20 1 calc PR A 2
C7A C 0.7154(15) 0.8473(14) 0.848(2) 0.063(6) Uani 0.20 1 d P A 2
H7A1 H 0.7200 0.8079 0.8885 0.095 Uiso 0.20 1 calc PR A 2
H7A2 H 0.6858 0.8621 0.8965 0.095 Uiso 0.20 1 calc PR A 2
H7A3 H 0.7652 0.8905 0.8353 0.095 Uiso 0.20 1 calc PR A 2
C8 C 0.5749(2) 0.6052(2) 0.8257(4) 0.0453(9) Uani 1 1 d . A .
C9 C 0.5494(2) 0.6212(2) 0.9468(3) 0.0439(8) Uani 1 1 d . A .
H9 H 0.5834 0.6201 1.0088 0.053 Uiso 1 1 calc R . .
C10 C 0.4685(2) 0.5612(2) 0.9809(3) 0.0483(9) Uani 1 1 d . . .
C11 C 0.4148(3) 0.5804(3) 1.0070(4) 0.0680(12) Uani 1 1 d . . .
H11 H 0.4266 0.6307 0.9990 0.082 Uiso 1 1 calc R . .
C12 C 0.3419(3) 0.5254(4) 1.0460(5) 0.0916(17) Uani 1 1 d . . .
H12 H 0.3062 0.5396 1.0657 0.110 Uiso 1 1 calc R . .
C13 C 0.3237(4) 0.4510(4) 1.0549(6) 0.102(2) Uani 1 1 d . . .
H13 H 0.2754 0.4142 1.0803 0.123 Uiso 1 1 calc R . .
C14 C 0.3757(4) 0.4312(3) 1.0269(6) 0.101(2) Uani 1 1 d . . .
H14 H 0.3628 0.3804 1.0324 0.121 Uiso 1 1 calc R . .
C15 C 0.4490(3) 0.4854(3) 0.9896(5) 0.0763(14) Uani 1 1 d . . .
H15 H 0.4845 0.4706 0.9708 0.092 Uiso 1 1 calc R . .
C16 C 0.9324(8) 0.8457(9) 0.7156(14) 0.160(5) Uani 0.67 1 d P . .
H16A H 0.8781 0.8220 0.7072 0.240 Uiso 0.67 1 calc PR . .
H16B H 0.9444 0.8338 0.7934 0.240 Uiso 0.67 1 calc PR . .
H16C H 0.9522 0.8272 0.6539 0.240 Uiso 0.67 1 calc PR . .
C17 C 0.9656(14) 0.9262(12) 0.704(2) 0.182(8) Uani 0.67 1 d P . .
N1 N 0.54347(17) 0.81261(17) 0.7267(3) 0.0469(7) Uani 1 1 d . . .
N2 N 0.67944(18) 0.82008(19) 0.7366(3) 0.0505(8) Uani 1 1 d . . .
O1 O 0.46219(13) 0.65622(13) 0.7253(2) 0.0454(6) Uani 1 1 d . . .
O2 O 0.59611(15) 0.65470(16) 0.7427(2) 0.0457(6) Uani 1 1 d . . .
O3 O 0.5768(2) 0.54503(17) 0.8161(3) 0.0735(9) Uani 1 1 d . . .
O4 O 0.55873(14) 0.69500(14) 0.9474(2) 0.0465(6) Uani 1 1 d D . .
O5 O 1.0347(14) 0.9645(14) 0.7116(17) 0.124(5) Uani 0.33 1 d P . .
Cu1 Cu 0.56712(2) 0.73314(2) 0.74874(5) 0.04029(12) Uani 1 1 d . A .
H1O H 0.5841(19) 0.713(2) 1.009(2) 0.049(11) Uiso 1 1 d 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
O1 C1 C2 122.4(3) . .
O1 C1 C2 118.1(3) . 3_565
C2 C1 C2 119.4(3) . 3_565
C3 C2 C1 122.3(3) . .
C3 C2 C1 117.1(3) . 2_665
C1 C2 C1 120.6(3) . 2_665
N1 C3 C2 126.8(3) . .
N1 C3 H3 116.6 . .
C2 C3 H3 116.6 . .
N1 C4 C5 108.2(4) . .
N1 C4 H4A 110.0 . .
C5 C4 H4A 110.0 . .
N1 C4 H4B 110.0 . .
C5 C4 H4B 110.0 . .
H4A C4 H4B 108.4 . .
C4 C5 N2 111.7(5) . .
C4 C5 H5A 109.3 . .
N2 C5 H5A 109.3 . .
C4 C5 H5B 109.3 . .
N2 C5 H5B 109.3 . .
H5A C5 H5B 107.9 . .
N2 C6 H6A 109.5 . .
N2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N2 C5A H5A1 109.6 . .
N2 C5A H5A2 109.6 . .
H5A1 C5A H5A2 108.1 . .
N2 C6A H6A1 109.5 . .
N2 C6A H6A2 109.5 . .
H6A1 C6A H6A2 109.5 . .
N2 C6A H6A3 109.5 . .
H6A1 C6A H6A3 109.5 . .
H6A2 C6A H6A3 109.5 . .
N2 C7A H7A1 109.5 . .
N2 C7A H7A2 109.5 . .
H7A1 C7A H7A2 109.5 . .
N2 C7A H7A3 109.5 . .
H7A1 C7A H7A3 109.5 . .
H7A2 C7A H7A3 109.5 . .
O3 C8 O2 123.3(4) . .
O3 C8 C9 117.5(3) . .
O2 C8 C9 119.1(3) . .
O4 C9 C10 111.4(3) . .
O4 C9 C8 110.4(3) . .
C10 C9 C8 113.1(3) . .
O4 C9 H9 107.2 . .
C10 C9 H9 107.2 . .
C8 C9 H9 107.2 . .
C11 C10 C15 118.5(4) . .
C11 C10 C9 121.5(4) . .
C15 C10 C9 120.0(4) . .
C10 C11 C12 121.1(5) . .
C10 C11 H11 119.5 . .
C12 C11 H11 119.5 . .
C13 C12 C11 119.7(6) . .
C13 C12 H12 120.2 . .
C11 C12 H12 120.2 . .
C14 C13 C12 119.7(6) . .
C14 C13 H13 120.2 . .
C12 C13 H13 120.2 . .
C13 C14 C15 121.4(6) . .
C13 C14 H14 119.3 . .
C15 C14 H14 119.3 . .
C10 C15 C14 119.6(6) . .
C10 C15 H15 120.2 . .
C14 C15 H15 120.2 . .
C17 C16 H16A 109.5 . .
C17 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C17 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O5 C17 O5 115(2) . 3_675
O5 C17 C16 117(3) . .
O5 C17 C16 127(2) 3_675 .
C3 N1 C4 119.2(3) . .
C3 N1 Cu1 126.0(3) . .
C4 N1 Cu1 114.7(3) . .
C7A N2 C6 134.7(12) . .
C7A N2 C5 69.5(12) . .
C6 N2 C5 115.0(6) . .
C7A N2 C7 38.5(11) . .
C6 N2 C7 109.5(6) . .
C5 N2 C7 107.0(5) . .
C7A N2 C5A 111.2(13) . .
C6 N2 C5A 72.9(9) . .
C5 N2 C5A 45.6(7) . .
C7 N2 C5A 140.6(7) . .
C7A N2 C6A 110(2) . .
C6 N2 C6A 35.8(19) . .
C5 N2 C6A 140(2) . .
C7 N2 C6A 76(2) . .
C5A N2 C6A 107(2) . .
C7A N2 Cu1 114.3(11) . .
C6 N2 Cu1 108.4(5) . .
C5 N2 Cu1 103.0(3) . .
C7 N2 Cu1 113.9(3) . .
C5A N2 Cu1 101.4(6) . .
C6A N2 Cu1 112.5(17) . .
C1 O1 Cu1 129.4(2) . .
C8 O2 Cu1 119.9(2) . .
C9 O4 Cu1 107.4(2) . .
C9 O4 H1O 102(3) . .
Cu1 O4 H1O 136(3) . .
C17 O5 C17 125(2) . 2_765
N1 Cu1 O1 91.38(11) . .
N1 Cu1 O2 170.37(13) . .
O1 Cu1 O2 89.80(11) . .
N1 Cu1 N2 84.66(13) . .
O1 Cu1 N2 168.24(13) . .
O2 Cu1 N2 92.31(12) . .
N1 Cu1 O4 113.31(12) . .
O1 Cu1 O4 89.48(10) . .
O2 Cu1 O4 76.26(10) . .
N2 Cu1 O4 102.26(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.290(4) .
C1 C2 1.422(5) .
C1 C2 1.441(5) 3_565
C2 C3 1.416(5) .
C2 C1 1.441(5) 2_665
C3 N1 1.293(5) .
C3 H3 0.9300 .
C4 N1 1.461(5) .
C4 C5 1.477(8) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N2 1.478(7) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 N2 1.417(10) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 N2 1.499(7) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C5A N2 1.550(16) .
C5A H5A1 0.9700 .
C5A H5A2 0.9700 .
C6A N2 1.58(4) .
C6A H6A1 0.9600 .
C6A H6A2 0.9600 .
C6A H6A3 0.9600 .
C7A N2 1.40(3) .
C7A H7A1 0.9600 .
C7A H7A2 0.9600 .
C7A H7A3 0.9600 .
C8 O3 1.244(4) .
C8 O2 1.268(4) .
C8 C9 1.531(5) .
C9 O4 1.412(4) .
C9 C10 1.522(5) .
C9 H9 0.9800 .
C10 C11 1.359(6) .
C10 C15 1.386(6) .
C11 C12 1.401(7) .
C11 H11 0.9300 .
C12 C13 1.366(10) .
C12 H12 0.9300 .
C13 C14 1.339(10) .
C13 H13 0.9300 .
C14 C15 1.397(8) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 C17 1.43(2) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 O5 1.22(2) .
C17 O5 1.32(2) 3_675
N1 Cu1 1.913(3) .
N2 Cu1 2.073(3) .
O1 Cu1 1.926(2) .
O2 Cu1 1.953(3) .
O4 Cu1 2.314(3) .
O4 H1O 0.819(5) .
O5 C17 1.32(2) 2_765
