#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:34:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179413 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/10/4331072.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_4331072
loop_
_publ_author_name
'Meng-Jung Tsai'
'Jing-Yun Wu'
'Ming-Hsi Chiang'
'Cheng-Hao Huang'
'Ming-Yu Kuo'
'Long-Li Lai'
_publ_section_title
;
 Infinite Copper(II) Coordination Architectures from a Resonative
 Aminotriazine-Derived Tripodal Ligand: Synthesis, Structures, and
 Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12360
_journal_page_last               12371
_journal_paper_doi               10.1021/ic3016854
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C25 H38 Cu2 N12 O14'
_chemical_formula_weight         857.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.448(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5146(12)
_cell_length_b                   25.643(3)
_cell_length_c                   13.6739(16)
_cell_measurement_reflns_used    4775
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.16
_cell_measurement_theta_min      2.58
_cell_volume                     3517.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22328
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS, 1996'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       needle
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0614
_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)+(0.0911P)²+11.1983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                4298
_reflns_number_total             6211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3016854_si_002_4.cif
_cod_data_source_block           cpd2
_cod_database_code               4331072
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cu1 Cu 0.63053(8) 0.87960(3) 0.67809(5) 0.0334(2) Uani 1 1 d .
Cu2 Cu 0.99522(7) 0.69250(3) 0.71426(5) 0.0309(2) Uani 1 1 d .
O1 O 0.5830(4) 0.91305(16) 0.5352(3) 0.0365(10) Uani 1 1 d .
O2 O 0.7984(4) 0.92213(17) 0.5991(3) 0.0400(10) Uani 1 1 d .
O3 O 0.6938(5) 0.95576(17) 0.4513(3) 0.0436(11) Uani 1 1 d .
O4 O 0.9458(4) 0.62837(15) 0.6250(3) 0.0361(10) Uani 1 1 d .
O5 O 1.1578(5) 0.63943(18) 0.6437(3) 0.0419(11) Uani 1 1 d .
O6 O 1.0518(5) 0.57455(19) 0.5540(4) 0.0555(14) Uani 1 1 d .
O7 O 0.5597(6) 0.7975(2) 0.1065(4) 0.0705(17) Uani 1 1 d .
O8 O 0.5983(8) 0.8761(3) 0.0744(5) 0.092(2) Uani 1 1 d .
O9 O 0.4939(6) 0.8242(2) -0.0504(5) 0.0711(17) Uani 1 1 d .
O10 O 0.6531(4) 0.81471(16) 0.6137(3) 0.0378(10) Uani 1 1 d .
H103 H 0.6747 0.7906 0.6570 0.057 Uiso 1 1 d R
H104 H 0.5954 0.8052 0.5593 0.057 Uiso 1 1 d R
O22 O 0.4140(5) 0.8648(2) 0.6609(4) 0.0516(12) Uani 1 1 d .
H105 H 0.4003 0.8846 0.7079 0.077 Uiso 1 1 d R
N1 N 0.8319(5) 0.80644(18) 0.9615(4) 0.0313(11) Uani 1 1 d .
H101 H 0.8409 0.8331 1.0011 0.038 Uiso 1 1 calc R
N2 N 0.8662(5) 0.71705(18) 0.9413(3) 0.0289(11) Uani 1 1 d .
N3 N 0.7568(5) 0.77097(18) 0.7970(4) 0.0300(11) Uani 1 1 d .
N4 N 0.7274(5) 0.85884(19) 0.8207(4) 0.0344(12) Uani 1 1 d .
N5 N 0.9375(5) 0.75512(18) 1.1023(4) 0.0327(11) Uani 1 1 d .
N6 N 0.7994(5) 0.68459(17) 0.7763(4) 0.0282(11) Uani 1 1 d .
H102 H 0.7233 0.6864 0.7258 0.042 Uiso 1 1 d R
N7 N 0.6230(5) 0.94848(19) 0.7409(4) 0.0367(12) Uani 1 1 d .
N8 N 1.0758(5) 0.74597(19) 1.2988(4) 0.0334(12) Uani 1 1 d .
N9 N 1.0559(5) 0.64093(19) 0.8311(4) 0.0316(11) Uani 1 1 d .
N10 N 0.6942(5) 0.93094(19) 0.5283(4) 0.0342(12) Uani 1 1 d .
N11 N 1.0571(6) 0.6134(2) 0.6072(4) 0.0389(13) Uani 1 1 d .
N12 N 0.5518(7) 0.8335(3) 0.0451(5) 0.0583(17) Uani 1 1 d .
C1 C 0.7703(6) 0.8125(2) 0.8577(5) 0.0310(13) Uani 1 1 d .
C2 C 0.8793(6) 0.7586(2) 1.0032(4) 0.0308(13) Uani 1 1 d .
C3 C 0.8077(6) 0.7261(2) 0.8419(4) 0.0303(13) Uani 1 1 d .
C4 C 0.7485(7) 0.9017(2) 0.8930(5) 0.0388(15) Uani 1 1 d .
H4A H 0.8434 0.9066 0.9249 0.047 Uiso 1 1 calc R
H4B H 0.7086 0.8933 0.9464 0.047 Uiso 1 1 calc R
C5 C 0.6886(6) 0.9515(2) 0.8411(5) 0.0364(14) Uani 1 1 d .
C6 C 0.6981(8) 0.9975(2) 0.8945(5) 0.0466(17) Uani 1 1 d .
H6 H 0.7464 0.9988 0.9637 0.056 Uiso 1 1 calc R
C7 C 0.6368(7) 1.0415(3) 0.8462(6) 0.0504(18) Uani 1 1 d .
H7 H 0.6408 1.0726 0.8818 0.060 Uiso 1 1 calc R
C8 C 0.5679(7) 1.0383(3) 0.7417(6) 0.0485(18) Uani 1 1 d .
H8 H 0.5269 1.0676 0.7060 0.058 Uiso 1 1 calc R
C9 C 0.5617(7) 0.9922(2) 0.6932(5) 0.0412(16) Uani 1 1 d .
H9 H 0.5133 0.9902 0.6241 0.049 Uiso 1 1 calc R
C10 C 0.9760(6) 0.7017(2) 1.1376(5) 0.0328(14) Uani 1 1 d .
H10A H 1.0337 0.6876 1.1005 0.039 Uiso 1 1 calc R
H10B H 0.8968 0.6801 1.1227 0.039 Uiso 1 1 calc R
C11 C 1.0466(6) 0.7000(2) 1.2499(5) 0.0301(13) Uani 1 1 d .
C12 C 1.0847(7) 0.6536(2) 1.3011(5) 0.0400(15) Uani 1 1 d .
H12 H 1.0640 0.6221 1.2663 0.048 Uiso 1 1 calc R
C13 C 1.1528(7) 0.6541(3) 1.4033(5) 0.0472(17) Uani 1 1 d .
H13 H 1.1773 0.6229 1.4388 0.057 Uiso 1 1 calc R
C14 C 1.1848(7) 0.7009(3) 1.4533(5) 0.0450(17) Uani 1 1 d .
H14 H 1.2332 0.7020 1.5225 0.054 Uiso 1 1 calc R
C15 C 1.1446(7) 0.7458(3) 1.3999(5) 0.0397(15) Uani 1 1 d .
H15 H 1.1650 0.7775 1.4340 0.048 Uiso 1 1 calc R
C16 C 0.8217(6) 0.6316(2) 0.8202(4) 0.0313(13) Uani 1 1 d .
H16A H 0.7822 0.6066 0.7664 0.038 Uiso 1 1 calc R
H16B H 0.7758 0.6284 0.8717 0.038 Uiso 1 1 calc R
C17 C 0.9641(6) 0.6178(2) 0.8674(4) 0.0310(13) Uani 1 1 d .
C18 C 1.0032(7) 0.5804(3) 0.9439(5) 0.0415(16) Uani 1 1 d .
H18 H 0.9400 0.5648 0.9696 0.050 Uiso 1 1 calc R
C19 C 1.1342(7) 0.5665(3) 0.9813(5) 0.0454(17) Uani 1 1 d .
H19 H 1.1606 0.5413 1.0324 0.054 Uiso 1 1 calc R
C20 C 1.2270(7) 0.5901(3) 0.9428(5) 0.0417(16) Uani 1 1 d .
H20 H 1.3166 0.5810 0.9667 0.050 Uiso 1 1 calc R
C21 C 1.1838(7) 0.6270(3) 0.8691(5) 0.0379(15) Uani 1 1 d .
H21 H 1.2463 0.6434 0.8438 0.046 Uiso 1 1 calc R
C22 C 0.3673(9) 0.8140(3) 0.6766(7) 0.069(2) Uani 1 1 d .
H22A H 0.4126 0.7882 0.6484 0.104 Uiso 1 1 calc R
H22B H 0.2731 0.8118 0.6431 0.104 Uiso 1 1 calc R
H22C H 0.3850 0.8078 0.7487 0.104 Uiso 1 1 calc R
C23 C 0.4809(9) 0.8021(3) 0.3472(7) 0.069(2) Uani 1 1 d .
H23A H 0.5058 0.8382 0.3527 0.103 Uiso 1 1 calc R
H23B H 0.3994 0.7976 0.2926 0.103 Uiso 1 1 calc R
H23C H 0.5501 0.7818 0.3332 0.103 Uiso 1 1 calc R
O23 O 0.4621(5) 0.7851(2) 0.4413(4) 0.0573(14) Uani 1 1 d .
H106 H 0.4579 0.7516 0.4439 0.086 Uiso 1 1 d R
C24 C 1.0024(10) 1.0001(3) 0.7769(6) 0.071(3) Uani 1 1 d .
H24A H 1.0750 1.0225 0.8120 0.106 Uiso 1 1 calc R
H24B H 0.9862 0.9753 0.8244 0.106 Uiso 1 1 calc R
H24C H 0.9238 1.0207 0.7484 0.106 Uiso 1 1 calc R
O24 O 1.0359(6) 0.9729(2) 0.6960(5) 0.0762(17) Uani 1 1 d .
H107 H 0.9597 0.9625 0.6499 0.114 Uiso 1 1 d R
C25 C 0.3512(11) 0.9516(6) 0.8490(7) 0.129(6) Uani 1 1 d .
H25A H 0.3943 0.9849 0.8538 0.194 Uiso 1 1 calc R
H25B H 0.4152 0.9257 0.8828 0.194 Uiso 1 1 calc R
H25C H 0.2818 0.9534 0.8813 0.194 Uiso 1 1 calc R
O25 O 0.2936(9) 0.9376(3) 0.7415(7) 0.118(3) Uani 1 1 d .
H108 H 0.2388 0.9649 0.7289 0.177 Uiso 1 1 d 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
O10 Cu1 N7 174.4(2) . .
O10 Cu1 N4 96.91(19) . .
N7 Cu1 N4 83.6(2) . .
O10 Cu1 O1 87.37(17) . .
N7 Cu1 O1 90.58(19) . .
N4 Cu1 O1 162.6(2) . .
O10 Cu1 O22 93.78(19) . .
N7 Cu1 O22 91.4(2) . .
N4 Cu1 O22 105.2(2) . .
O1 Cu1 O22 91.19(18) . .
N8 Cu2 N5 83.7(2) 4_575 4_575
N8 Cu2 O4 169.8(2) 4_575 .
N5 Cu2 O4 96.96(18) 4_575 .
N8 Cu2 N9 94.6(2) 4_575 .
N5 Cu2 N9 178.3(2) 4_575 .
O4 Cu2 N9 84.72(18) . .
N8 Cu2 N6 96.89(18) 4_575 .
N5 Cu2 N6 103.11(19) 4_575 .
O4 Cu2 N6 92.91(17) . .
N9 Cu2 N6 76.83(18) . .
N10 O1 Cu1 104.5(3) . .
N11 O4 Cu2 105.5(4) . .
C22 O22 Cu1 121.3(5) . .
C1 N1 C2 121.6(5) . .
C3 N2 C2 115.6(5) . .
C1 N3 C3 116.6(5) . .
C1 N4 C4 117.2(5) . .
C1 N4 Cu1 129.5(4) . .
C4 N4 Cu1 113.3(4) . .
C2 N5 C10 113.6(5) . .
C2 N5 Cu2 133.5(4) . 4_576
C10 N5 Cu2 112.7(4) . 4_576
C3 N6 C16 118.4(5) . .
C3 N6 Cu2 105.3(3) . .
C16 N6 Cu2 99.7(3) . .
C5 N7 C9 118.0(5) . .
C5 N7 Cu1 114.9(4) . .
C9 N7 Cu1 127.1(4) . .
C11 N8 C15 118.5(5) . .
C11 N8 Cu2 114.4(4) . 4_576
C15 N8 Cu2 126.9(4) . 4_576
C21 N9 C17 119.2(5) . .
C21 N9 Cu2 121.6(4) . .
C17 N9 Cu2 119.1(4) . .
O3 N10 O2 122.4(5) . .
O3 N10 O1 118.6(5) . .
O2 N10 O1 119.1(5) . .
O6 N11 O5 124.4(6) . .
O6 N11 O4 117.5(6) . .
O5 N11 O4 118.1(5) . .
O8 N12 O7 120.7(7) . .
O8 N12 O9 121.6(7) . .
O7 N12 O9 117.7(7) . .
N4 C1 N3 121.4(5) . .
N4 C1 N1 119.8(5) . .
N3 C1 N1 118.8(5) . .
N5 C2 N2 121.7(5) . .
N5 C2 N1 119.0(5) . .
N2 C2 N1 119.3(5) . .
N2 C3 N3 128.1(5) . .
N2 C3 N6 116.6(5) . .
N3 C3 N6 115.3(5) . .
N4 C4 C5 111.4(5) . .
N7 C5 C6 121.7(6) . .
N7 C5 C4 116.7(5) . .
C6 C5 C4 121.6(6) . .
C7 C6 C5 120.1(6) . .
C6 C7 C8 118.1(6) . .
C9 C8 C7 119.3(6) . .
C8 C9 N7 122.8(6) . .
N5 C10 C11 111.7(5) . .
N8 C11 C12 121.0(6) . .
N8 C11 C10 117.0(5) . .
C12 C11 C10 121.9(5) . .
C13 C12 C11 119.8(6) . .
C12 C13 C14 119.4(6) . .
C15 C14 C13 118.8(6) . .
N8 C15 C14 122.5(6) . .
N6 C16 C17 114.3(5) . .
N9 C17 C18 119.9(6) . .
N9 C17 C16 118.4(5) . .
C18 C17 C16 121.6(6) . .
C19 C18 C17 120.1(6) . .
C18 C19 C20 119.4(6) . .
C21 C20 C19 118.2(6) . .
N9 C21 C20 123.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O10 1.930(4) .
Cu1 N7 1.976(5) .
Cu1 N4 1.983(5) .
Cu1 O1 2.054(4) .
Cu1 O22 2.249(5) .
Cu2 N8 1.989(5) 4_575
Cu2 N5 1.990(5) 4_575
Cu2 O4 2.021(4) .
Cu2 N9 2.024(5) .
Cu2 N6 2.459(5) .
O1 N10 1.285(7) .
O2 N10 1.246(6) .
O3 N10 1.230(6) .
O4 N11 1.322(7) .
O5 N11 1.226(7) .
O6 N11 1.224(7) .
O7 N12 1.234(8) .
O8 N12 1.214(8) .
O9 N12 1.287(8) .
O22 C22 1.432(9) .
N1 C1 1.380(8) .
N1 C2 1.381(7) .
N2 C3 1.334(7) .
N2 C2 1.342(7) .
N3 C1 1.331(7) .
N3 C3 1.337(7) .
N4 C1 1.318(7) .
N4 C4 1.451(8) .
N5 C2 1.313(7) .
N5 C10 1.468(7) .
N5 Cu2 1.990(5) 4_576
N6 C3 1.379(7) .
N6 C16 1.477(7) .
N7 C5 1.338(8) .
N7 C9 1.359(8) .
N8 C11 1.346(7) .
N8 C15 1.354(8) .
N8 Cu2 1.989(5) 4_576
N9 C21 1.337(8) .
N9 C17 1.347(8) .
C4 C5 1.503(8) .
C5 C6 1.377(9) .
C6 C7 1.366(9) .
C7 C8 1.397(10) .
C8 C9 1.347(9) .
C10 C11 1.492(8) .
C11 C12 1.377(8) .
C12 C13 1.366(9) .
C13 C14 1.374(10) .
C14 C15 1.360(9) .
C16 C17 1.484(9) .
C17 C18 1.388(8) .
C18 C19 1.365(10) .
C19 C20 1.380(10) .
C20 C21 1.357(9) .
C23 O23 1.427(10) .
C24 O24 1.438(10) .
C25 O25 1.457(12) .
