#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:29:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179380 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/77/4327754.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_4327754
loop_
_publ_author_name
'Fengjuan Cui'
'Shaoguang Li'
'Chuandong Jia'
'Jennifer S. Mathieson'
'Leroy Cronin'
'Xiao-Juan Yang'
'Biao Wu'
_publ_section_title
;
 Anion-Dependent Formation of Helicates versus Mesocates of
 Triple-Stranded M2L3 (M = Fe2+, Cu2+) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              179
_journal_page_last               187
_journal_paper_doi               10.1021/ic201417y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C75 H63 Cu2 N21 O11'
_chemical_formula_weight         1561.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_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                   13.563(12)
_cell_length_b                   13.563(12)
_cell_length_c                   42.74(4)
_cell_measurement_reflns_used    2120
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      16.10
_cell_measurement_theta_min      2.58
_cell_volume                     6809(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            15111
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.9014
_exptl_absorpt_correction_T_min  0.8572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             2418
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5259
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0656
_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)+(0.0791P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                2903
_reflns_number_total             5259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201417y_si_002_6.cif
_cod_data_source_block           LCuNO3
_cod_original_cell_volume        6809(10)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4327754
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
N9 N 0.6667 0.3333 0.7664(17) 0.33(2) Uani 1 3 d S
O1 O 0.4397(7) 0.6874(13) 0.8150(3) 0.44(2) Uani 1 1 d D
Cu1 Cu 0.3333 0.6667 0.69604(3) 0.0748(4) Uani 1 3 d S
Cu2 Cu 0.3333 0.6667 0.96929(3) 0.0738(4) Uani 1 3 d S
O2 O 0.9713(7) 0.0751(7) 0.9044(2) 0.195(4) Uani 1 1 d .
O3 O 1.0000 0.0000 0.8690(4) 0.262(12) Uani 1 3 d S
O5 O 0.6945(8) 0.4361(7) 0.7577(2) 0.197(5) Uani 1 1 d .
N1 N 0.4756(5) 0.7806(5) 0.66835(14) 0.0821(15) Uani 1 1 d .
N2 N 0.4696(5) 0.6681(4) 0.72058(13) 0.0726(14) Uani 1 1 d .
N3 N 0.6111(5) 0.6058(5) 0.81439(12) 0.0761(14) Uani 1 1 d .
N4 N 0.6710(5) 0.7262(5) 0.85067(13) 0.0834(15) Uani 1 1 d .
N5 N 0.4686(4) 0.6651(4) 0.94457(13) 0.0724(14) Uani 1 1 d .
N6 N 0.3626(6) 0.5515(5) 0.99643(14) 0.0852(15) Uani 1 1 d .
N7 N 0.3333 0.6667 0.8206(9) 0.29(2) Uani 1 3 d SD
N8 N 1.0000 0.0000 0.8970(3) 0.102(4) Uani 1 3 d S
O4 O 0.6667 0.3333 0.8013(6) 0.294(18) Uani 1 3 d S
C1 C 0.4738(7) 0.8355(7) 0.6434(2) 0.098(2) Uani 1 1 d .
H1 H 0.4053 0.8344 0.6381 0.118 Uiso 1 1 calc R
C2 C 0.5658(11) 0.8934(8) 0.6251(2) 0.117(3) Uani 1 1 d .
H2 H 0.5587 0.9255 0.6060 0.141 Uiso 1 1 calc R
C3 C 0.6694(8) 0.9070(7) 0.6332(2) 0.105(3) Uani 1 1 d .
H3 H 0.7355 0.9533 0.6212 0.126 Uiso 1 1 calc R
C4 C 0.6747(9) 0.8503(7) 0.6601(2) 0.101(3) Uani 1 1 d .
H4 H 0.7437 0.8534 0.6660 0.122 Uiso 1 1 calc R
C5 C 0.5766(7) 0.7896(6) 0.67775(19) 0.079(2) Uani 1 1 d .
C6 C 0.5723(6) 0.7301(6) 0.70758(15) 0.0731(17) Uani 1 1 d .
C7 C 0.6639(6) 0.7296(8) 0.71808(17) 0.099(2) Uani 1 1 d .
H7 H 0.7350 0.7732 0.7078 0.118 Uiso 1 1 calc R
C8 C 0.6555(10) 0.6654(10) 0.7440(2) 0.128(3) Uani 1 1 d .
H8 H 0.7209 0.6641 0.7514 0.153 Uiso 1 1 calc R
C9 C 0.5519(8) 0.6024(7) 0.75950(17) 0.093(2) Uani 1 1 d .
C10 C 0.4629(6) 0.6101(6) 0.74624(17) 0.080(2) Uani 1 1 d .
H10 H 0.3909 0.5704 0.7563 0.096 Uiso 1 1 calc R
C11 C 0.5399(7) 0.5300(7) 0.78863(17) 0.095(2) Uani 1 1 d .
H11A H 0.4592 0.4871 0.7953 0.114 Uiso 1 1 calc R
H11B H 0.5647 0.4745 0.7835 0.114 Uiso 1 1 calc R
C12 C 0.7173(9) 0.6298(11) 0.8209(2) 0.144(4) Uani 1 1 d .
H12 H 0.7577 0.5996 0.8102 0.173 Uiso 1 1 calc R
C13 C 0.7570(6) 0.7022(9) 0.84451(19) 0.117(3) Uani 1 1 d .
H13 H 0.8281 0.7310 0.8549 0.140 Uiso 1 1 calc R
C14 C 0.5842(6) 0.6681(6) 0.83179(17) 0.0820(18) Uani 1 1 d D
H14 H 0.5156 0.6708 0.8310 0.098 Uiso 1 1 calc R
C15 C 0.6721(8) 0.8035(7) 0.87680(16) 0.096(2) Uani 1 1 d .
H15A H 0.6302 0.8422 0.8700 0.115 Uiso 1 1 calc R
H15B H 0.7516 0.8625 0.8815 0.115 Uiso 1 1 calc R
C16 C 0.6163(7) 0.7329(7) 0.90609(16) 0.095(2) Uani 1 1 d .
C17 C 0.6585(8) 0.6659(9) 0.92046(19) 0.111(3) Uani 1 1 d .
H17 H 0.7220 0.6633 0.9120 0.133 Uiso 1 1 calc R
C18 C 0.6036(8) 0.6048(8) 0.94717(18) 0.108(3) Uani 1 1 d .
H18 H 0.6328 0.5636 0.9580 0.130 Uiso 1 1 calc R
C19 C 0.5075(5) 0.6031(6) 0.95811(16) 0.0763(18) Uani 1 1 d .
C20 C 0.5180(6) 0.7254(6) 0.91957(16) 0.0758(17) Uani 1 1 d .
H20 H 0.4859 0.7662 0.9100 0.091 Uiso 1 1 calc R
C21 C 0.4521(6) 0.5457(7) 0.98752(18) 0.073(2) Uani 1 1 d .
C22 C 0.4864(8) 0.4847(8) 1.0043(2) 0.108(3) Uani 1 1 d .
H22 H 0.5514 0.4817 0.9973 0.129 Uiso 1 1 calc R
C23 C 0.4304(9) 0.4245(8) 1.0319(2) 0.109(3) Uani 1 1 d .
H23 H 0.4520 0.3782 1.0434 0.131 Uiso 1 1 calc R
C24 C 0.3404(8) 0.4408(8) 1.0403(2) 0.115(3) Uani 1 1 d .
H24 H 0.3013 0.4086 1.0593 0.138 Uiso 1 1 calc R
C25 C 0.3066(7) 0.5006(7) 1.02242(19) 0.100(2) Uani 1 1 d .
H25 H 0.2423 0.5063 1.0285 0.120 Uiso 1 1 calc R
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
O5 N9 O5 112(3) 2_655 .
O5 N9 O5 112(3) 2_655 3_665
O5 N9 O5 112(3) . 3_665
O5 N9 O4 106(3) 2_655 .
O5 N9 O4 106(3) . .
O5 N9 O4 106(3) 3_665 .
N2 Cu1 N2 97.6(2) 2_665 3_565
N2 Cu1 N2 97.6(2) 2_665 .
N2 Cu1 N2 97.6(2) 3_565 .
N2 Cu1 N1 92.6(2) 2_665 .
N2 Cu1 N1 169.5(2) 3_565 .
N2 Cu1 N1 78.4(2) . .
N2 Cu1 N1 78.4(2) 2_665 2_665
N2 Cu1 N1 92.6(2) 3_565 2_665
N2 Cu1 N1 169.5(2) . 2_665
N1 Cu1 N1 92.1(2) . 2_665
N2 Cu1 N1 169.5(2) 2_665 3_565
N2 Cu1 N1 78.4(2) 3_565 3_565
N2 Cu1 N1 92.6(2) . 3_565
N1 Cu1 N1 92.1(2) . 3_565
N1 Cu1 N1 92.1(2) 2_665 3_565
N5 Cu2 N5 97.4(2) . 2_665
N5 Cu2 N5 97.4(2) . 3_565
N5 Cu2 N5 97.4(2) 2_665 3_565
N5 Cu2 N6 77.6(2) . .
N5 Cu2 N6 169.6(2) 2_665 .
N5 Cu2 N6 92.3(2) 3_565 .
N5 Cu2 N6 169.6(2) . 3_565
N5 Cu2 N6 92.3(2) 2_665 3_565
N5 Cu2 N6 77.6(2) 3_565 3_565
N6 Cu2 N6 93.3(2) . 3_565
N5 Cu2 N6 92.3(2) . 2_665
N5 Cu2 N6 77.6(2) 2_665 2_665
N5 Cu2 N6 169.6(2) 3_565 2_665
N6 Cu2 N6 93.3(2) . 2_665
N6 Cu2 N6 93.3(2) 3_565 2_665
C1 N1 C5 119.3(7) . .
C1 N1 Cu1 126.8(5) . .
C5 N1 Cu1 113.8(5) . .
C10 N2 C6 117.3(6) . .
C10 N2 Cu1 127.1(5) . .
C6 N2 Cu1 115.5(4) . .
C14 N3 C12 109.8(6) . .
C14 N3 C11 125.0(6) . .
C12 N3 C11 124.8(6) . .
C14 N4 C13 110.4(6) . .
C14 N4 C15 124.0(6) . .
C13 N4 C15 125.5(6) . .
C20 N5 C19 120.7(6) . .
C20 N5 Cu2 125.0(5) . .
C19 N5 Cu2 114.1(4) . .
C21 N6 C25 121.2(7) . .
C21 N6 Cu2 113.7(6) . .
C25 N6 Cu2 124.6(6) . .
O1 N7 O1 116.9(10) . 2_665
O1 N7 O1 116.9(10) . 3_565
O1 N7 O1 116.9(10) 2_665 3_565
O3 N8 O2 104.0(8) . .
O3 N8 O2 104.0(8) . 3_765
O2 N8 O2 114.3(6) . 3_765
O3 N8 O2 104.0(8) . 2_645
O2 N8 O2 114.3(6) . 2_645
O2 N8 O2 114.3(6) 3_765 2_645
N1 C1 C2 122.2(8) . .
C1 C2 C3 121.3(8) . .
C2 C3 C4 117.8(9) . .
C5 C4 C3 118.3(9) . .
N1 C5 C4 120.7(8) . .
N1 C5 C6 115.7(7) . .
C4 C5 C6 123.5(8) . .
C7 C6 N2 122.8(7) . .
C7 C6 C5 120.6(7) . .
N2 C6 C5 116.2(6) . .
C6 C7 C8 119.6(8) . .
C7 C8 C9 120.6(8) . .
C10 C9 C8 114.2(7) . .
C10 C9 C11 124.0(8) . .
C8 C9 C11 121.8(8) . .
N2 C10 C9 125.4(7) . .
N3 C11 C9 109.4(6) . .
C13 C12 N3 109.2(7) . .
C12 C13 N4 104.0(7) . .
N3 C14 N4 106.4(5) . .
N4 C15 C16 109.7(6) . .
C20 C16 C17 116.3(7) . .
C20 C16 C15 122.3(8) . .
C17 C16 C15 121.3(8) . .
C18 C17 C16 117.8(8) . .
C19 C18 C17 120.7(8) . .
N5 C19 C18 121.0(7) . .
N5 C19 C21 116.6(6) . .
C18 C19 C21 121.9(7) . .
N5 C20 C16 123.3(7) . .
N6 C21 C22 119.9(8) . .
N6 C21 C19 117.4(7) . .
C22 C21 C19 122.6(8) . .
C21 C22 C23 123.2(9) . .
C24 C23 C22 112.4(8) . .
C25 C24 C23 122.6(8) . .
N6 C25 C24 120.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N9 O5 1.30(2) 2_655
N9 O5 1.30(2) .
N9 O5 1.30(2) 3_665
N9 O4 1.49(7) .
O1 N7 1.347(8) .
Cu1 N2 2.117(6) 2_665
Cu1 N2 2.117(6) 3_565
Cu1 N2 2.117(6) .
Cu1 N1 2.128(7) .
Cu1 N1 2.128(6) 2_665
Cu1 N1 2.128(6) 3_565
Cu2 N5 2.127(6) .
Cu2 N5 2.127(6) 2_665
Cu2 N5 2.127(6) 3_565
Cu2 N6 2.136(6) .
Cu2 N6 2.136(6) 3_565
Cu2 N6 2.136(7) 2_665
O2 N8 1.298(7) .
O3 N8 1.198(19) .
N1 C1 1.306(9) .
N1 C5 1.375(9) .
N2 C10 1.326(8) .
N2 C6 1.336(8) .
N3 C14 1.307(8) .
N3 C12 1.337(10) .
N3 C11 1.487(9) .
N4 C14 1.315(8) .
N4 C13 1.384(10) .
N4 C15 1.527(9) .
N5 C20 1.308(8) .
N5 C19 1.328(8) .
N6 C21 1.311(9) .
N6 C25 1.328(9) .
N7 O1 1.347(8) 2_665
N7 O1 1.347(8) 3_565
N8 O2 1.298(7) 3_765
N8 O2 1.298(7) 2_645
C1 C2 1.345(12) .
C2 C3 1.368(12) .
C3 C4 1.402(11) .
C4 C5 1.387(11) .
C5 C6 1.494(10) .
C6 C7 1.324(9) .
C7 C8 1.378(11) .
C8 C9 1.393(12) .
C9 C10 1.385(10) .
C9 C11 1.543(10) .
C12 C13 1.322(10) .
C15 C16 1.527(11) .
C16 C20 1.409(10) .
C16 C17 1.432(11) .
C17 C18 1.388(11) .
C18 C19 1.375(10) .
C19 C21 1.472(10) .
C21 C22 1.342(12) .
C22 C23 1.420(12) .
C23 C24 1.393(12) .
C24 C25 1.349(11) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.043 0.481 0.147 1979 741 ' '
