#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:14:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179833 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012965.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_7012965
loop_
_publ_author_name
'Christelle Gateau'
'Marinella Mazzanti'
'Jacques Pécaut'
'Frank A. Dunand'
'Lothar Helm'
_publ_section_title
;
 Solid-state and solution properties of the lanthanide complexes of a
 new nonadentate tripodal ligand derived from 1,4,7-triazacyclononane
;
_journal_issue                   12
_journal_name_full               'Dalton Trans.'
_journal_page_first              2428
_journal_page_last               2433
_journal_paper_doi               10.1039/b303079b
_journal_year                    2003
_chemical_formula_sum            'C27 H33 Lu N6 O9'
_chemical_formula_weight         760.56
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 99.6940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0084(6)
_cell_length_b                   11.8544(9)
_cell_length_c                   14.8334(12)
_cell_measurement_temperature    298(2)
_cell_volume                     1388.10(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7054
_diffrn_reflns_theta_full        28.85
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    3.622
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5165
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0316
_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)+(0.0435P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                4406
_reflns_number_total             5165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303079b.txt
_cod_data_source_block           complex_Lu(tpatcn)_(4)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      Pn
_cod_database_code               7012965
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu Lu 0.68294(4) 0.72385(2) 0.17968(3) 0.02099(8) Uani 1 1 d . . .
O11 O 0.4463(7) 0.6422(6) 0.0919(4) 0.0341(14) Uani 1 1 d . . .
O12 O 0.3224(8) 0.5685(6) -0.0406(5) 0.059(2) Uani 1 1 d . . .
O21 O 0.5350(7) 0.6929(5) 0.2970(4) 0.0364(14) Uani 1 1 d . . .
O22 O 0.4256(7) 0.5848(5) 0.3937(4) 0.0447(16) Uani 1 1 d . . .
O31 O 0.5191(7) 0.8852(4) 0.1586(4) 0.0318(13) Uani 1 1 d . . .
O32 O 0.4129(7) 1.0434(5) 0.2048(4) 0.0441(15) Uani 1 1 d . . .
N1 N 0.9299(7) 0.8238(6) 0.1168(4) 0.0271(14) Uani 1 1 d . . .
N2 N 0.8894(8) 0.5805(6) 0.1196(4) 0.0278(15) Uani 1 1 d . . .
N3 N 0.9712(9) 0.7070(6) 0.2900(5) 0.0298(16) Uani 1 1 d . . .
N11 N 0.6312(8) 0.7795(6) 0.0155(4) 0.0286(14) Uani 1 1 d . . .
N21 N 0.6476(8) 0.5202(6) 0.2147(4) 0.0309(15) Uani 1 1 d . . .
N31 N 0.7442(8) 0.8668(5) 0.3046(4) 0.0263(14) Uani 1 1 d . . .
C1 C 1.0299(11) 0.7493(6) 0.0651(6) 0.035(2) Uani 1 1 d . . .
H1A H 1.1413 0.7383 0.1014 0.042 Uiso 1 1 calc R . .
H1B H 1.0450 0.7875 0.0093 0.042 Uiso 1 1 calc R . .
C2 C 0.9526(12) 0.6352(8) 0.0404(6) 0.034(2) Uani 1 1 d . . .
H2A H 0.8591 0.6435 -0.0100 0.041 Uiso 1 1 calc R . .
H2B H 1.0366 0.5867 0.0202 0.041 Uiso 1 1 calc R . .
C3 C 1.0363(10) 0.5462(8) 0.1915(6) 0.038(2) Uani 1 1 d . . .
H3A H 1.1398 0.5764 0.1752 0.046 Uiso 1 1 calc R . .
H3B H 1.0454 0.4646 0.1918 0.046 Uiso 1 1 calc R . .
C4 C 1.0219(10) 0.5860(7) 0.2877(6) 0.0311(18) Uani 1 1 d . . .
H4A H 0.9389 0.5399 0.3112 0.037 Uiso 1 1 calc R . .
H4B H 1.1301 0.5755 0.3274 0.037 Uiso 1 1 calc R . .
C5 C 1.1077(10) 0.7843(7) 0.2667(6) 0.037(2) Uani 1 1 d . . .
H5A H 1.1929 0.7390 0.2444 0.044 Uiso 1 1 calc R . .
H5B H 1.1618 0.8216 0.3222 0.044 Uiso 1 1 calc R . .
C6 C 1.0442(10) 0.8738(7) 0.1955(5) 0.0328(19) Uani 1 1 d . . .
H6A H 0.9841 0.9319 0.2232 0.039 Uiso 1 1 calc R . .
H6B H 1.1400 0.9087 0.1743 0.039 Uiso 1 1 calc R . .
C11 C 0.8512(11) 0.9121(7) 0.0541(6) 0.034(2) Uani 1 1 d . . .
H11A H 0.9367 0.9493 0.0255 0.040 Uiso 1 1 calc R . .
H11B H 0.7983 0.9682 0.0877 0.040 Uiso 1 1 calc R . .
C12 C 0.7207(10) 0.8586(7) -0.0175(5) 0.0305(18) Uani 1 1 d . . .
C13 C 0.6947(11) 0.8862(8) -0.1099(6) 0.042(2) Uani 1 1 d . . .
H13A H 0.7565 0.9440 -0.1310 0.051 Uiso 1 1 calc R . .
C14 C 0.5792(13) 0.8283(10) -0.1685(6) 0.054(3) Uani 1 1 d . . .
H14A H 0.5633 0.8436 -0.2309 0.065 Uiso 1 1 calc R . .
C15 C 0.4837(13) 0.7452(8) -0.1347(6) 0.048(3) Uani 1 1 d . . .
H15A H 0.4030 0.7045 -0.1741 0.057 Uiso 1 1 calc R . .
C16 C 0.5108(12) 0.7237(8) -0.0405(6) 0.0324(18) Uani 1 1 d . . .
C17 C 0.4196(10) 0.6376(7) 0.0058(6) 0.0326(19) Uani 1 1 d . . .
C21 C 0.7881(16) 0.4799(11) 0.0874(9) 0.034(3) Uani 1 1 d . . .
H21A H 0.8629 0.4201 0.0741 0.041 Uiso 1 1 calc R . .
H21B H 0.7116 0.4980 0.0314 0.041 Uiso 1 1 calc R . .
C22 C 0.6854(14) 0.4386(7) 0.1595(5) 0.030(2) Uani 1 1 d . . .
C23 C 0.6325(11) 0.3281(7) 0.1641(7) 0.043(2) Uani 1 1 d . . .
H23A H 0.6665 0.2727 0.1267 0.051 Uiso 1 1 calc R . .
C24 C 0.5260(13) 0.3022(7) 0.2270(7) 0.048(3) Uani 1 1 d . . .
H24A H 0.4849 0.2294 0.2314 0.058 Uiso 1 1 calc R . .
C25 C 0.4832(12) 0.3883(8) 0.2828(6) 0.041(2) Uani 1 1 d . . .
H25A H 0.4143 0.3729 0.3259 0.050 Uiso 1 1 calc R . .
C26 C 0.5434(15) 0.4978(12) 0.2743(8) 0.030(3) Uani 1 1 d . . .
C27 C 0.4980(11) 0.5995(9) 0.3260(6) 0.032(2) Uani 1 1 d . . .
C31 C 0.9419(13) 0.7364(8) 0.3820(6) 0.035(2) Uani 1 1 d . . .
H31A H 0.8740 0.6781 0.4041 0.041 Uiso 1 1 calc R . .
H31B H 1.0497 0.7400 0.4232 0.041 Uiso 1 1 calc R . .
C32 C 0.8546(10) 0.8458(7) 0.3825(6) 0.0314(19) Uani 1 1 d . . .
C33 C 0.8748(11) 0.9182(7) 0.4543(5) 0.035(2) Uani 1 1 d . . .
H33A H 0.9520 0.9022 0.5069 0.042 Uiso 1 1 calc R . .
C34 C 0.7804(12) 1.0154(8) 0.4486(6) 0.044(2) Uani 1 1 d . . .
H34A H 0.7957 1.0669 0.4966 0.053 Uiso 1 1 calc R . .
C35 C 0.6620(11) 1.0363(7) 0.3708(6) 0.038(2) Uani 1 1 d . . .
H35A H 0.5946 1.1006 0.3664 0.046 Uiso 1 1 calc R . .
C36 C 0.6465(10) 0.9592(6) 0.2995(5) 0.0288(18) Uani 1 1 d . . .
C37 C 0.5164(10) 0.9658(7) 0.2147(5) 0.0294(18) Uani 1 1 d . . .
O1 O 0.3574(13) 0.8211(9) 0.4748(8) 0.127(5) Uani 1 1 d . . .
O2 O 0.7058(10) 0.6268(6) 0.5420(5) 0.065(2) Uani 1 1 d . . .
O3 O 0.6364(8) 0.8384(7) 0.6166(4) 0.0612(19) Uani 1 1 d . . .
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'
Lu Lu -0.4720 5.8584 '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
O21 Lu O31 83.2(2) . . ?
O21 Lu O11 83.2(2) . . ?
O31 Lu O11 83.0(2) . . ?
O21 Lu N11 139.7(2) . . ?
O31 Lu N11 69.6(2) . . ?
O11 Lu N11 64.9(2) . . ?
O21 Lu N21 66.2(2) . . ?
O31 Lu N21 138.3(2) . . ?
O11 Lu N21 66.6(2) . . ?
N11 Lu N21 117.0(2) . . ?
O21 Lu N31 66.9(2) . . ?
O31 Lu N31 64.84(19) . . ?
O11 Lu N31 137.6(2) . . ?
N11 Lu N31 121.7(2) . . ?
N21 Lu N31 121.1(2) . . ?
O21 Lu N3 91.6(2) . . ?
O31 Lu N3 124.9(2) . . ?
O11 Lu N3 151.0(3) . . ?
N11 Lu N3 128.3(2) . . ?
N21 Lu N3 85.1(2) . . ?
N31 Lu N3 62.8(2) . . ?
O21 Lu N1 149.7(2) . . ?
O31 Lu N1 91.3(2) . . ?
O11 Lu N1 125.8(2) . . ?
N11 Lu N1 62.7(2) . . ?
N21 Lu N1 129.3(2) . . ?
N31 Lu N1 83.7(2) . . ?
N3 Lu N1 67.3(2) . . ?
O21 Lu N2 126.0(2) . . ?
O31 Lu N2 149.82(19) . . ?
O11 Lu N2 92.4(2) . . ?
N11 Lu N2 81.4(2) . . ?
N21 Lu N2 62.9(2) . . ?
N31 Lu N2 129.3(2) . . ?
N3 Lu N2 67.8(2) . . ?
N1 Lu N2 67.3(2) . . ?
C17 O11 Lu 124.7(5) . . ?
C27 O21 Lu 126.1(6) . . ?
C37 O31 Lu 127.3(5) . . ?
C11 N1 C6 110.9(6) . . ?
C11 N1 C1 107.9(6) . . ?
C6 N1 C1 109.2(6) . . ?
C11 N1 Lu 106.2(4) . . ?
C6 N1 Lu 107.8(4) . . ?
C1 N1 Lu 114.8(5) . . ?
C21 N2 C2 109.5(8) . . ?
C21 N2 C3 109.4(8) . . ?
C2 N2 C3 110.2(6) . . ?
C21 N2 Lu 106.8(6) . . ?
C2 N2 Lu 107.5(5) . . ?
C3 N2 Lu 113.4(4) . . ?
C4 N3 C31 109.7(6) . . ?
C4 N3 C5 111.6(6) . . ?
C31 N3 C5 107.7(7) . . ?
C4 N3 Lu 106.0(5) . . ?
C31 N3 Lu 107.6(5) . . ?
C5 N3 Lu 114.1(5) . . ?
C12 N11 C16 120.0(7) . . ?
C12 N11 Lu 122.6(5) . . ?
C16 N11 Lu 117.4(6) . . ?
C22 N21 C26 119.5(8) . . ?
C22 N21 Lu 121.9(5) . . ?
C26 N21 Lu 115.7(7) . . ?
C36 N31 C32 119.3(7) . . ?
C36 N31 Lu 118.2(5) . . ?
C32 N31 Lu 121.8(5) . . ?
N1 C1 C2 115.1(7) . . ?
N2 C2 C1 112.0(7) . . ?
N2 C3 C4 113.9(6) . . ?
N3 C4 C3 112.5(7) . . ?
N3 C5 C6 114.3(7) . . ?
N1 C6 C5 111.0(7) . . ?
N1 C11 C12 108.7(7) . . ?
N11 C12 C13 122.1(8) . . ?
N11 C12 C11 113.2(7) . . ?
C13 C12 C11 124.7(8) . . ?
C14 C13 C12 119.3(9) . . ?
C13 C14 C15 119.2(8) . . ?
C16 C15 C14 119.1(9) . . ?
N11 C16 C15 120.2(9) . . ?
N11 C16 C17 114.3(7) . . ?
C15 C16 C17 125.4(8) . . ?
O12 C17 O11 124.6(9) . . ?
O12 C17 C16 120.2(8) . . ?
O11 C17 C16 115.1(7) . . ?
N2 C21 C22 111.2(9) . . ?
N21 C22 C23 123.6(9) . . ?
N21 C22 C21 113.6(8) . . ?
C23 C22 C21 122.8(9) . . ?
C22 C23 C24 117.8(9) . . ?
C25 C24 C23 118.3(8) . . ?
C26 C25 C24 120.3(9) . . ?
N21 C26 C25 120.4(11) . . ?
N21 C26 C27 114.1(11) . . ?
C25 C26 C27 125.5(10) . . ?
O22 C27 O21 124.9(9) . . ?
O22 C27 C26 118.7(9) . . ?
O21 C27 C26 116.4(8) . . ?
C32 C31 N3 111.4(7) . . ?
N31 C32 C33 121.9(8) . . ?
N31 C32 C31 113.6(7) . . ?
C33 C32 C31 124.5(8) . . ?
C32 C33 C34 119.4(8) . . ?
C33 C34 C35 119.5(8) . . ?
C34 C35 C36 118.5(8) . . ?
N31 C36 C35 121.3(8) . . ?
N31 C36 C37 114.1(7) . . ?
C35 C36 C37 124.5(8) . . ?
O32 C37 O31 124.7(8) . . ?
O32 C37 C36 120.0(7) . . ?
O31 C37 C36 115.2(7) . . ?
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
Lu O21 2.293(5) . ?
Lu O31 2.311(5) . ?
Lu O11 2.322(6) . ?
Lu N11 2.490(6) . ?
Lu N21 2.495(7) . ?
Lu N31 2.498(6) . ?
Lu N3 2.603(7) . ?
Lu N1 2.609(6) . ?
Lu N2 2.628(6) . ?
O11 C17 1.261(10) . ?
O12 C17 1.253(10) . ?
O21 C27 1.242(11) . ?
O22 C27 1.253(10) . ?
O31 C37 1.270(9) . ?
O32 C37 1.229(9) . ?
N1 C11 1.470(10) . ?
N1 C6 1.481(10) . ?
N1 C1 1.489(10) . ?
N2 C21 1.476(13) . ?
N2 C2 1.502(10) . ?
N2 C3 1.505(10) . ?
N3 C4 1.493(10) . ?
N3 C31 1.466(11) . ?
N3 C5 1.510(10) . ?
N11 C12 1.323(10) . ?
N11 C16 1.337(11) . ?
N21 C22 1.335(9) . ?
N21 C26 1.341(13) . ?
N31 C36 1.340(10) . ?
N31 C32 1.355(10) . ?
C1 C2 1.507(13) . ?
C3 C4 1.525(11) . ?
C5 C6 1.522(11) . ?
C11 C12 1.501(12) . ?
C12 C13 1.390(11) . ?
C13 C14 1.346(13) . ?
C14 C15 1.391(14) . ?
C15 C16 1.401(12) . ?
C16 C17 1.488(13) . ?
C21 C22 1.534(15) . ?
C22 C23 1.383(12) . ?
C23 C24 1.400(14) . ?
C24 C25 1.393(13) . ?
C25 C26 1.398(16) . ?
C26 C27 1.505(16) . ?
C31 C32 1.474(13) . ?
C32 C33 1.356(11) . ?
C33 C34 1.373(12) . ?
C34 C35 1.387(12) . ?
C35 C36 1.387(11) . ?
C36 C37 1.494(11) . ?
