#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:53:33 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180361 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/30/7203022.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_7203022
loop_
_publ_author_name
'Almesåker, Ann'
'Bourne, Susan A.'
'Ramon, Gaëlle'
'Scott, Janet L.'
'Strauss, Christopher R.'
_publ_section_title
;
 Coordination chemistry of N,N,4-tris(pyridin-2-ylmethyl)aniline: a
 novel flexible, multimodal ligand
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              997
_journal_paper_doi               10.1039/b708465j
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C24 H29 Cu N4 O8.25 S1.25'
_chemical_formula_sum            'C24 H29 Cu N4 O8.25 S1.25'
_chemical_formula_weight         609.13
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.7890(10)
_cell_angle_beta                 75.9070(10)
_cell_angle_gamma                71.3780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4677(2)
_cell_length_b                   10.1790(2)
_cell_length_c                   16.2431(4)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.7
_cell_volume                     1430.31(6)
_computing_cell_refinement       'Collect (Nonius (2000)'
_computing_data_collection       'Collect (Nonius (2000)'
_computing_data_reduction        'Collect (Nonius (2000)'
_computing_molecular_graphics    'WebLab ViewerPro (1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22892
_diffrn_reflns_theta_full        32.68
_diffrn_reflns_theta_max         32.68
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         10429
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0488
_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)+(0.0955P)²+0.9129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                9144
_reflns_number_total             10429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708465j.txt
_cod_data_source_block           c:\gaelle~1\articl~2\struct~2\(7)-cu~1\gr4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1430.32(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.03390(2) 0.07364(2) 0.073802(13) 0.01481(7) Uani 1 1 d . . .
N1 N 0.21514(17) 0.08741(15) 0.11387(9) 0.0149(2) Uani 1 1 d . . .
C14 C 0.1962(2) 0.26190(18) -0.01025(11) 0.0179(3) Uani 1 1 d . . .
N3 N 0.05730(18) 0.24548(16) -0.00068(10) 0.0176(3) Uani 1 1 d . . .
N2 N 0.05019(18) -0.08950(16) 0.16334(10) 0.0177(3) Uani 1 1 d . . .
C1 C 0.1656(2) 0.16858(17) 0.18747(11) 0.0159(3) Uani 1 1 d . . .
C8 C 0.1896(2) -0.13967(18) 0.18207(11) 0.0180(3) Uani 1 1 d . . .
C7 C 0.3003(2) -0.05994(18) 0.13761(12) 0.0187(3) Uani 1 1 d . . .
H7A H 0.3686 -0.0626 0.1758 0.022 Uiso 1 1 calc R . .
H7B H 0.3635 -0.1030 0.0857 0.022 Uiso 1 1 calc R . .
C18 C -0.0441(2) 0.33724(19) -0.04431(12) 0.0217(3) Uani 1 1 d . . .
H18 H -0.1424 0.3262 -0.0370 0.026 Uiso 1 1 calc R . .
C2 C 0.0118(2) 0.21504(19) 0.22400(12) 0.0198(3) Uani 1 1 d . . .
H2 H -0.0620 0.1987 0.1997 0.024 Uiso 1 1 calc R . .
C13 C 0.3033(2) 0.15296(19) 0.03814(11) 0.0182(3) Uani 1 1 d . . .
H13B H 0.3697 0.0809 0.0007 0.022 Uiso 1 1 calc R . .
H13A H 0.3687 0.1959 0.0570 0.022 Uiso 1 1 calc R . .
C3 C -0.0337(2) 0.2859(2) 0.29653(12) 0.0235(4) Uani 1 1 d . . .
H3 H -0.1389 0.3183 0.3209 0.028 Uiso 1 1 calc R . .
C12 C -0.0560(2) -0.1551(2) 0.20120(12) 0.0222(3) Uani 1 1 d . . .
H12 H -0.1551 -0.1185 0.1887 0.027 Uiso 1 1 calc R . .
C9 C 0.2298(3) -0.2602(2) 0.23693(13) 0.0247(4) Uani 1 1 d . . .
H9 H 0.3298 -0.2951 0.2483 0.030 Uiso 1 1 calc R . .
C11 C -0.0245(3) -0.2745(2) 0.25779(14) 0.0279(4) Uani 1 1 d . . .
H11 H -0.1013 -0.3184 0.2845 0.033 Uiso 1 1 calc R . .
C4 C 0.0719(3) 0.3097(2) 0.33347(12) 0.0244(4) Uani 1 1 d . . .
C17 C -0.0075(3) 0.4476(2) -0.09974(13) 0.0253(4) Uani 1 1 d . . .
H17 H -0.0804 0.5118 -0.1297 0.030 Uiso 1 1 calc R . .
C15 C 0.2399(2) 0.3696(2) -0.06539(13) 0.0235(4) Uani 1 1 d . . .
H15 H 0.3388 0.3791 -0.0718 0.028 Uiso 1 1 calc R . .
C6 C 0.2725(2) 0.1965(2) 0.22201(13) 0.0234(3) Uani 1 1 d . . .
H6 H 0.3773 0.1683 0.1961 0.028 Uiso 1 1 calc R . .
C10 C 0.1207(3) -0.3289(2) 0.27501(14) 0.0292(4) Uani 1 1 d . . .
H10 H 0.1455 -0.4122 0.3124 0.035 Uiso 1 1 calc R . .
C16 C 0.1358(3) 0.4630(2) -0.11082(13) 0.0276(4) Uani 1 1 d . . .
H16 H 0.1630 0.5369 -0.1493 0.033 Uiso 1 1 calc R . .
C5 C 0.2247(3) 0.2661(2) 0.29462(14) 0.0283(4) Uani 1 1 d . . .
H5 H 0.2980 0.2843 0.3183 0.034 Uiso 1 1 calc R . .
C19 C 0.0223(4) 0.3736(2) 0.41726(14) 0.0352(5) Uani 1 1 d . . .
H19B H 0.1069 0.4004 0.4287 0.042 Uiso 1 1 calc R . .
H19A H -0.0648 0.4584 0.4140 0.042 Uiso 1 1 calc R . .
C20 C -0.0231(4) 0.2683(2) 0.48837(14) 0.0365(6) Uani 1 1 d . . .
N4 N -0.1682(4) 0.2683(3) 0.51001(15) 0.0508(7) Uani 1 1 d . . .
H4N H -0.2371 0.3342 0.4863 0.075 Uiso 0.50 1 calc PR . .
C21 C 0.0833(4) 0.1685(3) 0.52697(17) 0.0463(7) Uani 1 1 d . . .
H21 H 0.1864 0.1697 0.5130 0.056 Uiso 1 1 calc R . .
C24 C -0.2110(5) 0.1674(4) 0.56850(19) 0.0569(9) Uani 1 1 d . . .
H24 H -0.3147 0.1683 0.5830 0.068 Uiso 1 1 calc R . .
C23 C -0.1065(6) 0.0652(3) 0.60639(17) 0.0583(11) Uani 1 1 d . . .
H23 H -0.1364 -0.0060 0.6465 0.070 Uiso 1 1 calc R . .
C22 C 0.0407(5) 0.0663(3) 0.58624(19) 0.0565(10) Uani 1 1 d . . .
H22 H 0.1145 -0.0035 0.6130 0.068 Uiso 1 1 calc R . .
O1A O -0.14564(14) 0.06675(14) 0.03727(9) 0.0191(2) Uani 1 1 d . . .
O3A O -0.27642(19) 0.2021(2) 0.15447(12) 0.0348(4) Uani 1 1 d . . .
O2A O -0.38241(18) 0.24468(17) 0.02693(11) 0.0288(3) Uani 1 1 d . . .
O4A O -0.38179(17) 0.03431(18) 0.12102(11) 0.0279(3) Uani 1 1 d . . .
O1 O 0.5399(4) -0.1010(4) 0.2853(2) 0.0609(10) Uani 0.72 1 d P . .
O2 O 0.5385(4) -0.5533(3) 0.2240(3) 0.0621(9) Uani 0.76 1 d P . .
O5 O -0.4032(5) 0.5012(4) -0.0816(4) 0.0572(12) Uani 0.55 1 d P . .
O4B O -0.6481(9) 0.4853(11) 0.5319(4) 0.051(3) Uani 0.25 1 d PD . .
O3B O -0.6111(10) 0.4618(10) 0.3853(5) 0.058(3) Uani 0.25 1 d PD . .
O1B O -0.3989(8) 0.4574(13) 0.4519(8) 0.083(5) Uani 0.25 1 d PD . .
O2B O -0.5191(19) 0.2663(10) 0.4722(11) 0.112(6) Uani 0.25 1 d PD . .
S1A S -0.30257(5) 0.13987(5) 0.08653(3) 0.02002(10) Uani 1 1 d . . .
S1B S -0.5515(4) 0.4151(3) 0.4565(2) 0.0456(6) Uani 0.25 1 d P . .
O3 O 0.3567(13) -0.0951(11) 0.6718(7) 0.059(3) Uani 0.24 1 d P . .
O6 O -0.4521(19) 0.029(3) 0.4214(7) 0.123(8) Uani 0.23 1 d P . .
O4 O -0.3476(4) -0.3843(4) 0.3031(2) 0.0580(8) Uani 0.76 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'
S S 0.1246 0.1234 '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
O1A Cu1 N3 96.45(6) . . ?
O1A Cu1 N2 98.51(6) . . ?
N3 Cu1 N2 164.66(7) . . ?
O1A Cu1 N1 177.81(6) . . ?
N3 Cu1 N1 82.76(6) . . ?
N2 Cu1 N1 82.17(6) . . ?
O1A Cu1 O1A 78.73(5) . 2 ?
N3 Cu1 O1A 93.16(6) . 2 ?
N2 Cu1 O1A 93.07(6) . 2 ?
N1 Cu1 O1A 103.33(5) . 2 ?
C1 N1 C13 112.72(13) . . ?
C1 N1 C7 111.12(14) . . ?
C13 N1 C7 111.66(14) . . ?
C1 N1 Cu1 111.03(11) . . ?
C13 N1 Cu1 105.21(10) . . ?
C7 N1 Cu1 104.64(10) . . ?
N3 C14 C15 121.90(17) . . ?
N3 C14 C13 115.96(15) . . ?
C15 C14 C13 122.06(17) . . ?
C14 N3 C18 119.41(16) . . ?
C14 N3 Cu1 112.86(12) . . ?
C18 N3 Cu1 127.59(13) . . ?
C8 N2 C12 119.26(16) . . ?
C8 N2 Cu1 112.50(12) . . ?
C12 N2 Cu1 128.14(14) . . ?
C6 C1 C2 119.77(17) . . ?
C6 C1 N1 120.18(16) . . ?
C2 C1 N1 120.03(15) . . ?
N2 C8 C9 122.03(17) . . ?
N2 C8 C7 115.76(15) . . ?
C9 C8 C7 122.17(17) . . ?
N1 C7 C8 109.32(14) . . ?
N3 C18 C17 121.34(19) . . ?
C1 C2 C3 119.65(18) . . ?
N1 C13 C14 109.63(14) . . ?
C4 C3 C2 121.14(19) . . ?
N2 C12 C11 121.7(2) . . ?
C8 C9 C10 118.6(2) . . ?
C12 C11 C10 119.07(19) . . ?
C3 C4 C5 118.35(18) . . ?
C3 C4 C19 120.5(2) . . ?
C5 C4 C19 121.0(2) . . ?
C16 C17 C18 119.29(19) . . ?
C16 C15 C14 118.48(19) . . ?
C5 C6 C1 119.50(19) . . ?
C11 C10 C9 119.27(19) . . ?
C17 C16 C15 119.57(18) . . ?
C6 C5 C4 121.5(2) . . ?
C20 C19 C4 109.05(18) . . ?
N4 C20 C21 119.8(3) . . ?
N4 C20 C19 119.0(3) . . ?
C21 C20 C19 121.1(3) . . ?
C20 N4 C24 120.6(3) . . ?
C20 C21 C22 119.8(4) . . ?
N4 C24 C23 120.6(4) . . ?
C22 C23 C24 119.1(3) . . ?
C23 C22 C21 120.0(3) . . ?
S1A O1A Cu1 118.48(8) . . ?
S1A O1A Cu1 140.16(8) . 2 ?
Cu1 O1A Cu1 101.27(5) . 2 ?
O1B O4B S1B 110.9(12) 2_466 . ?
O4B O1B S1B 148.9(14) 2_466 . ?
O4B O1B S1B 43.3(9) 2_466 2_466 ?
S1B O1B S1B 106.6(6) . 2_466 ?
O4A S1A O2A 110.79(10) . . ?
O4A S1A O3A 111.89(11) . . ?
O2A S1A O3A 112.23(11) . . ?
O4A S1A O1A 107.44(9) . . ?
O2A S1A O1A 107.91(9) . . ?
O3A S1A O1A 106.29(9) . . ?
O3B S1B O2B 109.8(7) . . ?
O3B S1B O4B 112.9(5) . . ?
O2B S1B O4B 112.1(8) . . ?
O3B S1B O1B 113.5(6) . . ?
O2B S1B O1B 109.2(7) . . ?
O4B S1B O1B 98.9(6) . . ?
O3B S1B O1B 119.8(5) . 2_466 ?
O2B S1B O1B 124.4(8) . 2_466 ?
O4B S1B O1B 25.8(5) . 2_466 ?
O1B S1B O1B 73.4(6) . 2_466 ?
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 O1A 1.9566(13) . ?
Cu1 N3 1.9846(15) . ?
Cu1 N2 1.9965(15) . ?
Cu1 N1 2.0292(15) . ?
Cu1 O1A 2.3314(13) 2 ?
N1 C1 1.470(2) . ?
N1 C13 1.490(2) . ?
N1 C7 1.491(2) . ?
C14 N3 1.347(2) . ?
C14 C15 1.392(2) . ?
C14 C13 1.496(3) . ?
N3 C18 1.349(2) . ?
N2 C8 1.344(2) . ?
N2 C12 1.348(2) . ?
C1 C6 1.392(3) . ?
C1 C2 1.391(2) . ?
C8 C9 1.387(3) . ?
C8 C7 1.499(2) . ?
C18 C17 1.389(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.384(3) . ?
C12 C11 1.384(3) . ?
C9 C10 1.391(3) . ?
C11 C10 1.386(4) . ?
C4 C5 1.390(3) . ?
C4 C19 1.518(3) . ?
C17 C16 1.380(3) . ?
C15 C16 1.388(3) . ?
C6 C5 1.389(3) . ?
C19 C20 1.510(3) . ?
C20 N4 1.333(4) . ?
C20 C21 1.367(4) . ?
N4 C24 1.362(4) . ?
C21 C22 1.377(5) . ?
C24 C23 1.361(6) . ?
C23 C22 1.355(6) . ?
O1A S1A 1.5257(14) . ?
O1A Cu1 2.3314(13) 2 ?
O3A S1A 1.4701(16) . ?
O2A S1A 1.4567(17) . ?
O4A S1A 1.4586(16) . ?
O4B O1B 0.940(15) 2_466 ?
O4B S1B 1.482(8) . ?
O3B S1B 1.354(8) . ?
O1B O4B 0.940(15) 2_466 ?
O1B S1B 1.616(10) . ?
O1B S1B 2.018(16) 2_466 ?
O2B S1B 1.434(10) . ?
S1B O1B 2.018(16) 2_466 ?
O3 O6 1.71(2) 2_556 ?
O6 O3 1.71(2) 2_556 ?
