#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:07:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179776 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007230.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_7007230
loop_
_publ_author_name
'Farrell, David'
'Harding, Charles J.'
'McKee, Vickie'
'Nelson, Jane'
_publ_section_title
;
 Effect of methylation on the coordination of copper by small
 azacryptands; the role of geometrically constrained hydrogen bonding
 in stabilizing terminally coordinated oxygen species.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3204
_journal_page_last               3211
_journal_paper_doi               10.1039/b602003h
_journal_year                    2006
_chemical_formula_sum            'C24 H57 Cl3 Cu N8 O13'
_chemical_formula_weight         835.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           155
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :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                   10.1113(12)
_cell_length_b                   10.1113(12)
_cell_length_c                   29.655(5)
_cell_measurement_reflns_used    2695
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.44
_cell_measurement_theta_min      2.42
_cell_volume                     2625.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            6242
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.574600
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1323
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0367
_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)+(0.0579P)²+2.8152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                972
_reflns_number_total             1042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602003h.txt
_cod_data_source_block           4_(cume6)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      R32
_cod_database_code               7007230
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+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
Cu1 Cu 0.3333 0.6667 0.12025(5) 0.0229(3) Uani 0.50 3 d SP . .
O1 O 0.3333 0.6667 0.1827(3) 0.0226(12) Uani 0.50 3 d SP . .
N1 N 0.3333 0.6667 0.05140(12) 0.0285(8) Uani 1 3 d S . .
C1 C 0.2672(5) 0.5063(3) 0.03598(9) 0.0342(8) Uani 1 1 d . . .
H1A H 0.3003 0.5049 0.0046 0.041 Uiso 1 1 calc R . .
H1B H 0.1544 0.4559 0.0362 0.041 Uiso 1 1 calc R . .
C2 C 0.3178(4) 0.4191(4) 0.06625(10) 0.0325(8) Uani 1 1 d . . .
H2A H 0.2762 0.3141 0.0545 0.039 Uiso 1 1 calc R . .
H2B H 0.4306 0.4694 0.0657 0.039 Uiso 1 1 calc R . .
N3 N 0.2657(3) 0.4118(3) 0.11338(9) 0.0325(6) Uani 1 1 d . . .
C3 C 0.3499(4) 0.3545(4) 0.14163(9) 0.0335(7) Uani 1 1 d . . .
H3A H 0.4607 0.4249 0.1375 0.040 Uiso 1 1 calc R . .
H3B H 0.3266 0.2536 0.1297 0.040 Uiso 1 1 calc R . .
C4 C 0.1009(4) 0.3050(6) 0.11654(14) 0.0536(11) Uani 1 1 d . . .
H4A H 0.0672 0.3016 0.1477 0.080 Uiso 1 1 calc R . .
H4B H 0.0789 0.2028 0.1074 0.080 Uiso 1 1 calc R . .
H4C H 0.0465 0.3392 0.0967 0.080 Uiso 1 1 calc R . .
Cl1 Cl -0.3333 0.3333 0.09378(3) 0.0260(3) Uani 1 3 d S . .
O11 O -0.3333 0.3333 0.14215(11) 0.0377(8) Uani 1 3 d S . .
O12 O -0.3152(3) 0.4759(3) 0.07741(8) 0.0399(6) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.0000 0.0000 0.0462(5) Uani 1 6 d S . .
O21 O 0.0000 0.0000 0.0508(3) 0.101(4) Uani 0.50 3 d SP . .
O22 O 0.1075(8) -0.0456(9) -0.0126(3) 0.087(3) Uani 0.50 1 d P . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 Cu1 O1 0.0 10_455 . ?
O1 Cu1 N1 180.0 10_455 . ?
O1 Cu1 N1 180.000(1) . . y
O1 Cu1 N3 95.03(8) 10_455 3_565 ?
O1 Cu1 N3 95.03(7) . 3_565 ?
N1 Cu1 N3 84.97(7) . 3_565 ?
O1 Cu1 N3 95.03(7) 10_455 2_665 ?
O1 Cu1 N3 95.03(8) . 2_665 ?
N1 Cu1 N3 84.97(7) . 2_665 ?
N3 Cu1 N3 119.24(2) 3_565 2_665 ?
O1 Cu1 N3 95.04(7) 10_455 . ?
O1 Cu1 N3 95.03(7) . . y
N1 Cu1 N3 84.97(7) . . y
N3 Cu1 N3 119.24(2) 3_565 . ?
N3 Cu1 N3 119.24(2) 2_665 . ?
O1 Cu1 Cu1 0.0 10_455 10_455 ?
O1 Cu1 Cu1 0.0 . 10_455 ?
N1 Cu1 Cu1 180.0 . 10_455 ?
N3 Cu1 Cu1 95.03(7) 3_565 10_455 ?
N3 Cu1 Cu1 95.03(7) 2_665 10_455 ?
N3 Cu1 Cu1 95.03(7) . 10_455 ?
Cu1 O1 O1 180.0 10_455 10_455 ?
Cu1 O1 Cu1 180.0 10_455 . ?
O1 O1 Cu1 0.0 10_455 . ?
C1 N1 C1 110.96(16) 3_565 2_665 ?
C1 N1 C1 110.96(16) 3_565 . ?
C1 N1 C1 110.96(16) 2_665 . ?
C1 N1 Cu1 107.94(17) 3_565 . ?
C1 N1 Cu1 107.94(17) 2_665 . ?
C1 N1 Cu1 107.94(17) . . ?
N1 C1 C2 110.8(3) . . ?
N3 C2 C1 111.9(3) . . ?
C4 N3 C2 110.0(3) . . ?
C4 N3 C3 109.6(3) . . ?
C2 N3 C3 106.8(2) . . ?
C4 N3 Cu1 114.0(2) . . ?
C2 N3 Cu1 97.30(19) . . ?
C3 N3 Cu1 118.0(2) . . ?
N3 C3 C3 117.0(3) . 12 ?
O11 Cl1 O12 109.66(11) . 3_455 ?
O11 Cl1 O12 109.66(11) . 2_565 ?
O12 Cl1 O12 109.28(11) 3_455 2_565 ?
O11 Cl1 O12 109.66(11) . . ?
O12 Cl1 O12 109.28(11) 3_455 . ?
O12 Cl1 O12 109.28(11) 2_565 . ?
O22 Cl2 O22 113.4(3) 3 2 ?
O22 Cl2 O22 154.6(6) 3 5 ?
O22 Cl2 O22 90.5(6) 2 5 ?
O22 Cl2 O22 90.5(6) 3 4 ?
O22 Cl2 O22 45.1(6) 2 4 ?
O22 Cl2 O22 113.4(3) 5 4 ?
O22 Cl2 O22 45.1(6) 3 6 ?
O22 Cl2 O22 154.6(6) 2 6 ?
O22 Cl2 O22 113.4(3) 5 6 ?
O22 Cl2 O22 113.4(3) 4 6 ?
O22 Cl2 O22 113.4(3) 3 . ?
O22 Cl2 O22 113.4(3) 2 . ?
O22 Cl2 O22 45.1(6) 5 . ?
O22 Cl2 O22 154.6(6) 4 . ?
O22 Cl2 O22 90.5(6) 6 . ?
O22 Cl2 O21 105.2(3) 3 . ?
O22 Cl2 O21 105.2(3) 2 . ?
O22 Cl2 O21 74.8(3) 5 . ?
O22 Cl2 O21 74.8(3) 4 . ?
O22 Cl2 O21 74.8(3) 6 . ?
O22 Cl2 O21 105.2(3) . . ?
O22 Cl2 O21 74.8(3) 3 4 ?
O22 Cl2 O21 74.8(3) 2 4 ?
O22 Cl2 O21 105.2(3) 5 4 ?
O22 Cl2 O21 105.2(3) 4 4 ?
O22 Cl2 O21 105.2(3) 6 4 ?
O22 Cl2 O21 74.8(3) . 4 ?
O21 Cl2 O21 180.0 . 4 ?
Cl2 O21 O22 50.6(3) . 6 ?
Cl2 O21 O22 50.6(3) . 4 ?
O22 O21 O22 84.0(5) 6 4 ?
Cl2 O21 O22 50.6(3) . 5 ?
O22 O21 O22 84.0(5) 6 5 ?
O22 O21 O22 84.0(5) 4 5 ?
O22 O22 Cl2 67.4(3) 5 . ?
O22 O22 O21 105.7(7) 5 4 ?
Cl2 O22 O21 54.6(4) . 4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 0.902(7) 10_455 ?
Cu1 O1 1.851(9) . y
Cu1 N1 2.042(4) . y
Cu1 N3 2.322(3) 3_565 ?
Cu1 N3 2.322(3) 2_665 ?
Cu1 N3 2.322(3) . y
Cu1 Cu1 2.753(3) 10_455 ?
O1 Cu1 0.902(7) 10_455 ?
O1 O1 0.948(16) 10_455 ?
N1 C1 1.484(3) 3_565 ?
N1 C1 1.484(3) 2_665 ?
N1 C1 1.484(3) . ?
C1 C2 1.515(5) . ?
C2 N3 1.482(4) . ?
N3 C4 1.467(5) . ?
N3 C3 1.501(4) . ?
C3 C3 1.513(6) 12 ?
Cl1 O11 1.434(3) . ?
Cl1 O12 1.444(2) 3_455 ?
Cl1 O12 1.444(2) 2_565 ?
Cl1 O12 1.444(2) . ?
Cl2 O22 1.427(6) 3 ?
Cl2 O22 1.427(6) 2 ?
Cl2 O22 1.427(6) 5 ?
Cl2 O22 1.427(6) 4 ?
Cl2 O22 1.427(6) 6 ?
Cl2 O22 1.427(6) . ?
Cl2 O21 1.505(10) . ?
Cl2 O21 1.505(10) 4 ?
O21 O22 1.782(10) 6 ?
O21 O22 1.782(10) 4 ?
O21 O22 1.782(10) 5 ?
O22 O22 1.094(14) 5 ?
O22 O21 1.782(10) 4 ?
