#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:53:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180361 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/30/7203020.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_7203020
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         '[Cu(tpma-H)(NO32](NO3)'
_chemical_formula_sum            'C24 H23 Cu N7 O9'
_chemical_formula_weight         617.03
_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                93.94(3)
_cell_angle_beta                 92.29(3)
_cell_angle_gamma                116.16(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0308(16)
_cell_length_b                   8.6296(17)
_cell_length_c                   20.091(4)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.1
_cell_volume                     1242.9(5)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9603
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plates
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.411
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.411
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0648
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                4139
_reflns_number_total             4392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708465j.txt
_cod_data_source_block           c:\gaelle~1\articl~2\struct~2\(5)-cu~1\gr2
_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        1242.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203020
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 0.25191(6) 0.66051(6) 0.84418(3) 0.0171(2) Uani 1 1 d . . .
N2 N 0.2527(5) 0.8566(5) 0.80131(18) 0.0189(8) Uani 1 1 d . . .
O2A O 0.1648(5) 0.4567(5) 0.7409(2) 0.0430(10) Uani 1 1 d . . .
O1B O 0.3332(6) 0.8370(6) 0.9464(2) 0.0466(11) Uani 1 1 d . . .
C4 C 0.6633(6) 0.6184(6) 0.6355(2) 0.0204(9) Uani 1 1 d . . .
N1 N 0.5453(5) 0.7845(4) 0.82496(17) 0.0156(7) Uani 1 1 d . . .
O3A O -0.1253(4) 0.2678(4) 0.72935(17) 0.0305(8) Uani 1 1 d . . .
N1B N 0.1778(5) 0.8035(5) 0.96505(19) 0.0217(8) Uani 1 1 d . . .
N3 N 0.3223(5) 0.5004(5) 0.88838(18) 0.0207(8) Uani 1 1 d . . .
N1A N 0.0030(6) 0.3963(5) 0.7594(2) 0.0278(9) Uani 1 1 d . . .
O3B O 0.1654(6) 0.8697(5) 1.01944(19) 0.0446(10) Uani 1 1 d . . .
C14 C 0.5072(6) 0.5540(5) 0.8983(2) 0.0168(9) Uani 1 1 d . . .
C6 C 0.5841(7) 0.8141(6) 0.7040(2) 0.0263(11) Uani 1 1 d . . .
H2 H 0.5556 0.9100 0.7072 0.032 Uiso 1 1 calc R . .
C1 C 0.5832(5) 0.7278(5) 0.7607(2) 0.0168(9) Uani 1 1 d . . .
C8 C 0.4211(6) 0.9905(6) 0.8005(2) 0.0170(9) Uani 1 1 d . . .
C7 C 0.5826(6) 0.9707(5) 0.8317(2) 0.0175(9) Uani 1 1 d . . .
H7A H 0.6965 1.0403 0.8096 0.021 Uiso 1 1 calc R . .
H7B H 0.6036 1.0143 0.8797 0.021 Uiso 1 1 calc R . .
C16 C 0.4556(7) 0.2858(6) 0.9414(2) 0.0249(10) Uani 1 1 d . . .
H16 H 0.5009 0.2110 0.9590 0.030 Uiso 1 1 calc R . .
C18 C 0.2045(7) 0.3446(6) 0.9060(2) 0.0242(10) Uani 1 1 d . . .
H18 H 0.0745 0.3095 0.9001 0.029 Uiso 1 1 calc R . .
O2C O 1.3843(6) 0.9537(6) 0.5895(2) 0.0534(12) Uani 1 1 d . . .
C2 C 0.6180(6) 0.5848(6) 0.7529(2) 0.0204(9) Uani 1 1 d . . .
H6 H 0.6146 0.5219 0.7902 0.025 Uiso 1 1 calc R . .
C10 C 0.2873(6) 1.1510(6) 0.7446(2) 0.0246(10) Uani 1 1 d . . .
H10 H 0.2998 1.2528 0.7255 0.030 Uiso 1 1 calc R . .
O1A O -0.0232(6) 0.4743(5) 0.8107(2) 0.0422(10) Uani 1 1 d . . .
C5 C 0.6267(6) 0.7597(6) 0.6429(2) 0.0233(10) Uani 1 1 d . . .
H3 H 0.6306 0.8219 0.6054 0.028 Uiso 1 1 calc R . .
C13 C 0.6302(6) 0.7374(5) 0.8826(2) 0.0182(9) Uani 1 1 d . . .
H13B H 0.6486 0.8192 0.9224 0.022 Uiso 1 1 calc R . .
H13A H 0.7536 0.7473 0.8719 0.022 Uiso 1 1 calc R . .
C9 C 0.4430(6) 1.1397(6) 0.7722(2) 0.0215(9) Uani 1 1 d . . .
H9 H 0.5633 1.2336 0.7716 0.026 Uiso 1 1 calc R . .
O1C O 1.1122(6) 0.9516(6) 0.5820(2) 0.0535(12) Uani 1 1 d . . .
C15 C 0.5785(6) 0.4483(6) 0.9242(2) 0.0205(9) Uani 1 1 d . . .
H15 H 0.7091 0.4866 0.9301 0.025 Uiso 1 1 calc R . .
C20 C 0.8317(6) 0.4760(6) 0.5733(2) 0.0228(10) Uani 1 1 d . . .
C12 C 0.1008(6) 0.8666(6) 0.7740(2) 0.0241(10) Uani 1 1 d . . .
H12 H -0.0182 0.7708 0.7745 0.029 Uiso 1 1 calc R . .
N1C N 1.2834(7) 1.0225(6) 0.5739(2) 0.0393(11) Uani 1 1 d . . .
O3C O 1.3530(7) 1.1657(6) 0.5473(3) 0.0657(14) Uani 1 1 d . . .
C3 C 0.6578(6) 0.5315(6) 0.6915(2) 0.0207(9) Uani 1 1 d . . .
H5 H 0.6819 0.4330 0.6877 0.025 Uiso 1 1 calc R . .
C11 C 0.1151(7) 1.0125(7) 0.7456(2) 0.0276(11) Uani 1 1 d . . .
H11 H 0.0072 1.0172 0.7268 0.033 Uiso 1 1 calc R . .
N4 N 1.0167(6) 0.5718(7) 0.5886(2) 0.0404(11) Uani 1 1 d . . .
H4N H 1.0652 0.6855 0.5955 0.048 Uiso 1 1 calc R . .
C21 C 0.7587(8) 0.3021(6) 0.5627(2) 0.0327(12) Uani 1 1 d . . .
H21 H 0.6287 0.2351 0.5520 0.039 Uiso 1 1 calc R . .
C17 C 0.2655(7) 0.2343(6) 0.9323(2) 0.0269(10) Uani 1 1 d . . .
H17 H 0.1789 0.1243 0.9440 0.032 Uiso 1 1 calc R . .
O2B O 0.0439(7) 0.7055(7) 0.9274(2) 0.0808(19) Uani 1 1 d . . .
C19 C 0.7065(7) 0.5612(7) 0.5682(2) 0.0308(12) Uani 1 1 d . . .
H19A H 0.5884 0.4795 0.5427 0.037 Uiso 1 1 calc R . .
H19B H 0.7655 0.6637 0.5427 0.037 Uiso 1 1 calc R . .
C24 C 1.1292(10) 0.4868(16) 0.5933(3) 0.082(3) Uani 1 1 d . . .
H24 H 1.2594 0.5508 0.6043 0.098 Uiso 1 1 calc R . .
C23 C 1.049(2) 0.309(2) 0.5817(5) 0.133(7) Uani 1 1 d . . .
H23 H 1.1226 0.2482 0.5841 0.160 Uiso 1 1 calc R . .
C22 C 0.869(2) 0.2239(12) 0.5672(4) 0.101(4) Uani 1 1 d . . .
H22 H 0.8143 0.1010 0.5596 0.121 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
_geom_angle_publ_flag
N2 Cu1 N3 164.85(16) . . ?
N2 Cu1 O1A 98.25(15) . . ?
N3 Cu1 O1A 96.12(16) . . ?
N2 Cu1 N1 82.06(14) . . ?
N3 Cu1 N1 83.22(14) . . ?
O1A Cu1 N1 147.73(15) . . ?
N2 Cu1 O1B 87.57(15) . . ?
N3 Cu1 O1B 88.28(14) . . ?
O1A Cu1 O1B 124.39(15) . . ?
N1 Cu1 O1B 87.87(14) . . ?
C8 N2 C12 119.6(4) . . ?
C8 N2 Cu1 114.6(3) . . ?
C12 N2 Cu1 125.8(3) . . ?
N1B O1B Cu1 100.6(3) . . ?
C3 C4 C5 117.5(4) . . ?
C3 C4 C19 122.0(4) . . ?
C5 C4 C19 120.4(4) . . ?
C1 N1 C13 113.8(3) . . ?
C1 N1 C7 113.6(3) . . ?
C13 N1 C7 112.8(3) . . ?
C1 N1 Cu1 113.8(3) . . ?
C13 N1 Cu1 101.2(2) . . ?
C7 N1 Cu1 100.4(2) . . ?
O2B N1B O3B 123.8(5) . . ?
O2B N1B O1B 117.1(5) . . ?
O3B N1B O1B 119.1(4) . . ?
C14 N3 C18 119.5(4) . . ?
C14 N3 Cu1 114.6(3) . . ?
C18 N3 Cu1 125.8(3) . . ?
O3A N1A O2A 121.9(4) . . ?
O3A N1A O1A 121.2(4) . . ?
O2A N1A O1A 117.0(4) . . ?
N3 C14 C15 121.3(4) . . ?
N3 C14 C13 116.1(4) . . ?
C15 C14 C13 122.6(4) . . ?
C5 C6 C1 120.2(4) . . ?
C2 C1 C6 117.8(4) . . ?
C2 C1 N1 120.8(4) . . ?
C6 C1 N1 121.4(4) . . ?
N2 C8 C9 121.0(4) . . ?
N2 C8 C7 116.7(4) . . ?
C9 C8 C7 122.3(4) . . ?
N1 C7 C8 110.4(3) . . ?
C17 C16 C15 119.0(4) . . ?
N3 C18 C17 122.2(5) . . ?
C3 C2 C1 121.1(4) . . ?
C11 C10 C9 119.0(4) . . ?
N1A O1A Cu1 102.3(3) . . ?
C4 C5 C6 121.8(4) . . ?
N1 C13 C14 110.9(3) . . ?
C8 C9 C10 119.5(4) . . ?
C14 C15 C16 119.0(4) . . ?
C21 C20 N4 120.2(5) . . ?
C21 C20 C19 119.2(5) . . ?
N4 C20 C19 120.5(5) . . ?
N2 C12 C11 121.6(4) . . ?
O2C N1C O1C 121.3(5) . . ?
O2C N1C O3C 119.5(5) . . ?
O1C N1C O3C 119.1(5) . . ?
C2 C3 C4 121.6(4) . . ?
C12 C11 C10 119.3(4) . . ?
C20 N4 C24 118.8(6) . . ?
C20 C21 C22 119.9(7) . . ?
C18 C17 C16 119.1(4) . . ?
C20 C19 C4 113.3(4) . . ?
C23 C24 N4 119.0(8) . . ?
C22 C23 C24 119.1(7) . . ?
C23 C22 C21 123.0(9) . . ?
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 N2 1.948(4) . ?
Cu1 N3 1.958(4) . ?
Cu1 O1A 2.126(4) . ?
Cu1 N1 2.180(4) . ?
Cu1 O1B 2.355(5) . ?
N2 C8 1.338(6) . ?
N2 C12 1.357(6) . ?
O2A N1A 1.251(6) . ?
O1B N1B 1.231(5) . ?
C4 C3 1.386(6) . ?
C4 C5 1.374(6) . ?
C4 C19 1.514(6) . ?
N1 C1 1.440(5) . ?
N1 C13 1.490(5) . ?
N1 C7 1.494(5) . ?
O3A N1A 1.228(5) . ?
N1B O2B 1.220(6) . ?
N1B O3B 1.226(5) . ?
N3 C14 1.348(6) . ?
N3 C18 1.341(6) . ?
N1A O1A 1.268(6) . ?
C14 C15 1.390(6) . ?
C14 C13 1.515(6) . ?
C6 C5 1.392(6) . ?
C6 C1 1.402(6) . ?
C1 C2 1.381(6) . ?
C8 C9 1.386(6) . ?
C8 C7 1.501(6) . ?
C16 C17 1.390(7) . ?
C16 C15 1.390(6) . ?
C18 C17 1.372(7) . ?
O2C N1C 1.240(6) . ?
C2 C3 1.384(6) . ?
C10 C11 1.374(7) . ?
C10 C9 1.392(6) . ?
O1C N1C 1.257(6) . ?
C20 C21 1.346(7) . ?
C20 N4 1.353(6) . ?
C20 C19 1.489(6) . ?
C12 C11 1.379(7) . ?
N1C O3C 1.276(7) . ?
N4 C24 1.397(10) . ?
C21 C22 1.331(12) . ?
C24 C23 1.377(16) . ?
C23 C22 1.308(18) . ?
