#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:32:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179975 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/69/7026937.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_7026937
loop_
_publ_author_name
'Ebrahimpour, Parisa'
'Cushion, Michael'
'Haddow, Mairi F.'
'Hallett, Andrew J.'
'Wass, Duncan F.'
_publ_section_title
;
 Cu(I) complexes based on cis, cis-1,3,5-tris(arylideneamino)cyclohexane
 ligands: synthesis, structure and CO binding.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10910
_journal_page_last               10919
_journal_paper_doi               10.1039/c0dt00986e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C33 H39 N3 O6, 6(H2 O)'
_chemical_formula_sum            'C33 H51 N3 O12'
_chemical_formula_weight         681.77
_chemical_name_common            5.1
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_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            6
_cell_length_a                   21.4700(7)
_cell_length_b                   21.4700(7)
_cell_length_c                   13.9509(10)
_cell_measurement_temperature    100(2)
_cell_volume                     5569.3(5)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33104
_diffrn_reflns_theta_full        32.54
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2197.21
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0911P)²+4.6323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                3081
_reflns_number_total             4476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00986e.txt
_cod_data_source_block           5.1_0m
_cod_original_sg_symbol_H-M      'R -3 '
_cod_database_code               7026937
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'
'-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
O1 O 0.30039(6) 0.13145(6) -0.00118(8) 0.0299(2) Uani 1 1 d .
O2 O 0.22282(6) -0.02576(6) 0.26083(8) 0.0322(3) Uani 1 1 d .
N1 N 0.14226(6) 0.02510(6) 0.17164(8) 0.0200(2) Uani 1 1 d .
C1 C 0.06030(7) 0.07317(7) 0.16974(9) 0.0205(2) Uani 1 1 d .
H1A H 0.0622 0.0755 0.2406 0.025 Uiso 1 1 calc R
H1B H 0.0987 0.1198 0.1446 0.025 Uiso 1 1 calc R
C2 C 0.07312(6) 0.01281(7) 0.13555(9) 0.0188(2) Uani 1 1 d .
H2 H 0.0743 0.0130 0.0639 0.023 Uiso 1 1 calc R
C3 C 0.19098(7) 0.04001(7) 0.10941(9) 0.0205(2) Uani 1 1 d .
H3 H 0.1793 0.0412 0.0440 0.025 Uiso 1 1 calc R
C4 C 0.26419(7) 0.05555(7) 0.13209(9) 0.0219(2) Uani 1 1 d .
C5 C 0.32089(7) 0.10442(7) 0.07314(10) 0.0246(3) Uani 1 1 d .
C6 C 0.39201(8) 0.12247(8) 0.09185(12) 0.0318(3) Uani 1 1 d .
H6 H 0.4303 0.1560 0.0525 0.038 Uiso 1 1 calc R
C7 C 0.40522(8) 0.09040(9) 0.16891(13) 0.0342(3) Uani 1 1 d .
H7 H 0.4535 0.1028 0.1824 0.041 Uiso 1 1 calc R
C8 C 0.35089(8) 0.04083(9) 0.22719(12) 0.0318(3) Uani 1 1 d .
H8 H 0.3617 0.0191 0.2790 0.038 Uiso 1 1 calc R
C9 C 0.28005(7) 0.02325(8) 0.20885(10) 0.0247(3) Uani 1 1 d .
C10 C 0.23634(11) -0.06040(11) 0.33903(13) 0.0431(4) Uani 1 1 d .
H10A H 0.2587 -0.0875 0.3149 0.065 Uiso 1 1 calc R
H10B H 0.1909 -0.0934 0.3708 0.065 Uiso 1 1 calc R
H10C H 0.2687 -0.0241 0.3850 0.065 Uiso 1 1 calc R
C11 C 0.35473(10) 0.18019(9) -0.06573(13) 0.0395(4) Uani 1 1 d .
H11A H 0.3899 0.2229 -0.0305 0.059 Uiso 1 1 calc R
H11B H 0.3325 0.1946 -0.1159 0.059 Uiso 1 1 calc R
H11C H 0.3790 0.1565 -0.0950 0.059 Uiso 1 1 calc R
O3 O 0.54066(8) 0.19236(9) 0.91665(9) 0.0454(3) Uani 1 1 d .
H12 H 0.5132(10) 0.1626(10) 0.8517(14) 0.027(4) Uiso 1 1 d .
H13 H 0.5418(14) 0.1467(15) 0.9146(19) 0.063(7) Uiso 1 1 d .
O4 O 0.53780(6) 0.31974(8) 0.95530(8) 0.0363(3) Uani 1 1 d .
H14 H 0.5379(12) 0.2769(14) 0.9525(16) 0.048(6) Uiso 1 1 d .
H15 H 0.5234(14) 0.3181(14) 1.019(2) 0.063(7) 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'
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
C5 O1 C11 118.11(13) . .
C9 O2 C10 117.99(12) . .
C3 N1 C2 116.36(10) . .
C2 C1 C2 110.69(11) 2 .
C2 C1 H1A 109.5 2 .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 2 .
C2 C1 H1B 109.5 . .
H1A C1 H1B 108.1 . .
N1 C2 C1 109.86(10) . 3
N1 C2 C1 109.66(10) . .
C1 C2 C1 110.77(12) 3 .
N1 C2 H2 108.8 . .
C1 C2 H2 108.8 3 .
C1 C2 H2 108.8 . .
N1 C3 C4 124.23(11) . .
N1 C3 H3 117.9 . .
C4 C3 H3 117.9 . .
C9 C4 C5 118.66(12) . .
C9 C4 C3 123.18(12) . .
C5 C4 C3 118.16(12) . .
O1 C5 C6 124.30(13) . .
O1 C5 C4 114.72(12) . .
C6 C5 C4 120.98(14) . .
C7 C6 C5 118.37(14) . .
C7 C6 H6 120.8 . .
C5 C6 H6 120.8 . .
C6 C7 C8 122.48(13) . .
C6 C7 H7 118.8 . .
C8 C7 H7 118.8 . .
C7 C8 C9 119.10(14) . .
C7 C8 H8 120.5 . .
C9 C8 H8 120.5 . .
O2 C9 C8 123.54(13) . .
O2 C9 C4 116.06(11) . .
C8 C9 C4 120.39(14) . .
O2 C10 H10A 109.5 . .
O2 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O2 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O1 C11 H11A 109.5 . .
O1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
O1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
H12 O3 H13 70.9(17) . .
H14 O4 H15 100(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C5 1.3642(18) .
O1 C11 1.4305(18) .
O2 C9 1.3602(18) .
O2 C10 1.4297(18) .
N1 C3 1.2712(16) .
N1 C2 1.4611(15) .
C1 C2 1.5278(17) 2
C1 C2 1.5295(17) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C1 1.5279(17) 3
C2 H2 1.0000 .
C3 C4 1.4687(18) .
C3 H3 0.9500 .
C4 C9 1.4071(19) .
C4 C5 1.4078(19) .
C5 C6 1.399(2) .
C6 C7 1.380(3) .
C6 H6 0.9500 .
C7 C8 1.383(2) .
C7 H7 0.9500 .
C8 C9 1.3953(19) .
C8 H8 0.9500 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
O3 H12 1.096(19) .
O3 H13 0.99(3) .
O4 H14 0.92(3) .
O4 H15 0.94(3) .
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_4
C3 N1 C2 C1 125.42(12) . 3
C3 N1 C2 C1 -112.61(12) . .
C2 C1 C2 N1 -178.21(8) 2 .
C2 C1 C2 C1 -56.79(16) 2 3
C2 N1 C3 C4 178.63(11) . .
N1 C3 C4 C9 33.0(2) . .
N1 C3 C4 C5 -147.88(13) . .
C11 O1 C5 C6 1.5(2) . .
C11 O1 C5 C4 -178.54(13) . .
C9 C4 C5 O1 178.08(11) . .
C3 C4 C5 O1 -1.04(17) . .
C9 C4 C5 C6 -1.98(19) . .
C3 C4 C5 C6 178.90(12) . .
O1 C5 C6 C7 -179.17(13) . .
C4 C5 C6 C7 0.9(2) . .
C5 C6 C7 C8 0.7(2) . .
C6 C7 C8 C9 -1.1(2) . .
C10 O2 C9 C8 0.7(2) . .
C10 O2 C9 C4 179.48(14) . .
C7 C8 C9 O2 178.73(13) . .
C7 C8 C9 C4 0.0(2) . .
C5 C4 C9 O2 -177.30(12) . .
C3 C4 C9 O2 1.77(19) . .
C5 C4 C9 C8 1.53(19) . .
C3 C4 C9 C8 -179.40(13) . .
