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#$Date: 2021-07-05 11:57:19 +0300 (Mon, 05 Jul 2021) $
#$Revision: 266989 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/39/1563928.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_1563928
loop_
_publ_author_name
'Molloy, Jennifer K.'
'Fedele, Lionel'
'Jarjayes, Olivier'
'Philouze, Christian'
'Imbert, Daniel'
'Thomas, Fabrice'
_publ_section_title
;
 Structural and spectroscopic investigations of redox active seven
 coordinate luminescent lanthanide complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              609
_journal_page_last               617
_journal_paper_doi               10.1016/j.ica.2018.08.054
_journal_volume                  483
_journal_year                    2018
_chemical_formula_moiety         'C51 H75 Lu1 N4 O3, 1.5(C2 H3 N)'
_chemical_formula_sum            'C54 H79.5 Lu N5.5 O3'
_chemical_formula_weight         1028.70
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.514(3)
_cell_length_b                   27.514(3)
_cell_length_c                   27.514(3)
_cell_measurement_reflns_used    24942
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.480
_cell_volume                     20829(4)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2016 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Incoatec-Bruker-AXS-enraf-noniusKappaAPEXII
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24942
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         1.480
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.311439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1597 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.3114.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             8592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0176P)²+81.6005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2352
_reflns_number_total             3071
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2018-483-609.cif
_cod_data_source_block           Lu
_cod_original_cell_volume        20829(7)
_cod_original_formula_sum        'C54 H79.50 Lu N5.50 O3'
_cod_database_code               1563928
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C36(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) N5(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C34(H34A,H34B,
 H34C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.12783(2) 0.12783(2) 0.12783(2) 0.02409(10) Uani 1 3 d S T P . .
C1 C 0.12955(13) 0.13909(13) 0.01054(13) 0.0242(8) Uani 1 1 d . . . . .
N1 N 0.13769(12) 0.20819(11) 0.09486(12) 0.0303(7) Uani 1 1 d . . . . .
C2 C 0.12288(14) 0.19020(13) 0.00936(14) 0.0278(8) Uani 1 1 d . . . . .
O1 O 0.13998(10) 0.11727(9) 0.05142(9) 0.0302(6) Uani 1 1 d . . . . .
C6 C 0.12655(13) 0.11264(13) -0.03413(13) 0.0260(8) Uani 1 1 d . . . . .
C7 C 0.13080(14) 0.22103(14) 0.05070(14) 0.0295(8) Uani 1 1 d . . . . .
H7 H 0.130927 0.255006 0.044534 0.035 Uiso 1 1 calc R . . . .
C22 C 0.14931(16) 0.24655(14) 0.12993(15) 0.0362(10) Uani 1 1 d . . . . .
H22A H 0.121392 0.251980 0.151971 0.043 Uiso 1 1 calc R . . . .
H22B H 0.156295 0.277340 0.112667 0.043 Uiso 1 1 calc R . . . .
C33 C 0.13121(17) 0.03682(16) -0.08692(15) 0.0414(11) Uani 1 1 d . . . . .
H33A H 0.097594 0.040856 -0.097973 0.062 Uiso 1 1 calc GR . . . .
H33B H 0.139449 0.002172 -0.086365 0.062 Uiso 1 1 calc GR . . . .
H33C H 0.153160 0.053884 -0.109187 0.062 Uiso 1 1 calc GR . . . .
C28 C 0.09390(15) 0.21302(15) -0.12577(15) 0.0347(9) Uani 1 1 d . . . . .
N4 N 0.18407(12) 0.18407(12) 0.18407(12) 0.0317(13) Uani 1 3 d S T P . .
C32 C 0.13658(15) 0.05800(14) -0.03570(14) 0.0309(9) Uani 1 1 d . . . . .
C4 C 0.10666(14) 0.18896(14) -0.07749(14) 0.0314(9) Uani 1 1 d . . . . .
C3 C 0.11158(14) 0.21387(14) -0.03462(14) 0.0316(9) Uani 1 1 d . . . . .
H3 H 0.107236 0.248127 -0.034569 0.038 Uiso 1 1 calc R . . . .
C5 C 0.11504(14) 0.13834(14) -0.07575(14) 0.0300(8) Uani 1 1 d . . . . .
H5 H 0.112590 0.120680 -0.105316 0.036 Uiso 1 1 calc R . . . .
C23 C 0.19321(16) 0.23081(15) 0.15876(16) 0.0391(10) Uani 1 1 d . . . . .
H23A H 0.221357 0.227138 0.136647 0.047 Uiso 1 1 calc R . . . .
H23B H 0.201325 0.256146 0.182991 0.047 Uiso 1 1 calc R . . . .
C29 C 0.08014(18) 0.26667(16) -0.11942(17) 0.0482(12) Uani 1 1 d . . . . .
H29A H 0.052948 0.269324 -0.096563 0.072 Uiso 1 1 calc GR . . . .
H29B H 0.070554 0.280281 -0.150904 0.072 Uiso 1 1 calc GR . . . .
H29C H 0.108121 0.284682 -0.106718 0.072 Uiso 1 1 calc GR . . . .
C35 C 0.18900(16) 0.04845(16) -0.01881(17) 0.0437(11) Uani 1 1 d . . . . .
H35A H 0.211759 0.064055 -0.041331 0.066 Uiso 1 1 calc GR . . . .
H35B H 0.195072 0.013355 -0.018222 0.066 Uiso 1 1 calc GR . . . .
H35C H 0.193573 0.061840 0.013872 0.066 Uiso 1 1 calc GR . . . .
C34 C 0.10140(17) 0.02997(15) -0.00266(17) 0.0426(11) Uani 1 1 d . . . . .
H34A H 0.103587 0.042704 0.030532 0.064 Uiso 1 1 calc GR . . . .
H34B H 0.110039 -0.004582 -0.002717 0.064 Uiso 1 1 calc GR . . . .
H34C H 0.068114 0.033906 -0.014715 0.064 Uiso 1 1 calc GR . . . .
C30 C 0.05058(17) 0.18710(18) -0.14942(18) 0.0465(11) Uani 1 1 d . . . . .
H30A H 0.059740 0.153648 -0.157522 0.070 Uiso 1 1 calc GR . . . .
H30B H 0.041197 0.204366 -0.179131 0.070 Uiso 1 1 calc GR . . . .
H30C H 0.023135 0.186736 -0.126728 0.070 Uiso 1 1 calc GR . . . .
C31 C 0.13818(17) 0.20992(17) -0.15990(16) 0.0449(11) Uani 1 1 d . . . . .
H31A H 0.165110 0.228742 -0.146155 0.067 Uiso 1 1 calc GR . . . .
H31B H 0.129520 0.223151 -0.191819 0.067 Uiso 1 1 calc GR . . . .
H31C H 0.148077 0.175886 -0.163452 0.067 Uiso 1 1 calc GR . . . .
C36 C 0.2494(4) 0.2106(4) 0.0194(4) 0.062(3) Uani 0.5 1 d . . . A -1
C37 C 0.2460(5) 0.1726(5) -0.0159(5) 0.075(5) Uani 0.5 1 d . . . A -1
H37A H 0.226449 0.183802 -0.043533 0.113 Uiso 0.5 1 calc GR . . A -1
H37B H 0.230464 0.144120 -0.001197 0.113 Uiso 0.5 1 calc GR . . A -1
H37C H 0.278595 0.163873 -0.027202 0.113 Uiso 0.5 1 calc GR . . A -1
N5 N 0.2526(5) 0.2386(5) 0.0475(5) 0.113(5) Uani 0.5 1 d . . . A -1
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
N1 Lu1 N1 106.59(9) 9 5
N1 Lu1 N1 106.58(9) 9 .
N1 Lu1 N1 106.59(9) 5 .
N1 Lu1 N4 67.78(8) 9 .
N1 Lu1 N4 67.78(8) 5 .
N1 Lu1 N4 67.78(8) . .
O1 Lu1 N1 85.20(11) 9 5
O1 Lu1 N1 74.80(10) 5 5
O1 Lu1 N1 166.77(11) 5 9
O1 Lu1 N1 74.80(10) 9 9
O1 Lu1 N1 85.20(11) . 9
O1 Lu1 N1 74.80(10) . .
O1 Lu1 N1 166.77(11) . 5
O1 Lu1 N1 85.21(11) 5 .
O1 Lu1 N1 166.77(11) 9 .
O1 Lu1 O1 92.35(10) 9 .
O1 Lu1 O1 92.35(10) 5 .
O1 Lu1 O1 92.35(10) 5 9
O1 Lu1 N4 123.59(7) . .
O1 Lu1 N4 123.59(7) 5 .
O1 Lu1 N4 123.59(7) 9 .
C2 C1 C6 118.5(3) . .
O1 C1 C2 120.2(3) . .
O1 C1 C6 121.2(3) . .
C7 N1 Lu1 126.5(3) . .
C7 N1 C22 117.3(3) . .
C22 N1 Lu1 116.0(2) . .
C1 C2 C7 123.2(3) . .
C3 C2 C1 120.4(3) . .
C3 C2 C7 116.2(3) . .
C1 O1 Lu1 138.2(2) . .
C1 C6 C32 120.9(3) . .
C5 C6 C1 117.7(3) . .
C5 C6 C32 121.4(3) . .
N1 C7 C2 127.7(4) . .
N1 C7 H7 116.1 . .
C2 C7 H7 116.1 . .
N1 C22 H22A 110.0 . .
N1 C22 H22B 110.0 . .
N1 C22 C23 108.3(3) . .
H22A C22 H22B 108.4 . .
C23 C22 H22A 110.0 . .
C23 C22 H22B 110.0 . .
H33A C33 H33B 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C32 C33 H33A 109.5 . .
C32 C33 H33B 109.5 . .
C32 C33 H33C 109.5 . .
C4 C28 C29 112.0(4) . .
C4 C28 C30 110.3(3) . .
C4 C28 C31 109.0(3) . .
C29 C28 C31 108.5(4) . .
C30 C28 C29 107.7(4) . .
C30 C28 C31 109.3(4) . .
C23 N4 Lu1 109.1(3) 5 .
C23 N4 Lu1 109.1(3) 9 .
C23 N4 Lu1 109.1(3) . .
C23 N4 C23 109.8(3) . 9
C23 N4 C23 109.8(3) . 5
C23 N4 C23 109.8(3) 9 5
C6 C32 C33 112.5(3) . .
C6 C32 C35 109.2(3) . .
C6 C32 C34 111.3(3) . .
C33 C32 C35 107.7(3) . .
C33 C32 C34 107.0(3) . .
C34 C32 C35 109.1(4) . .
C3 C4 C28 123.7(4) . .
C3 C4 C5 116.6(4) . .
C5 C4 C28 119.7(4) . .
C2 C3 H3 119.0 . .
C4 C3 C2 122.0(4) . .
C4 C3 H3 119.0 . .
C6 C5 C4 124.7(4) . .
C6 C5 H5 117.6 . .
C4 C5 H5 117.6 . .
C22 C23 H23A 109.4 . .
C22 C23 H23B 109.4 . .
N4 C23 C22 111.1(3) . .
N4 C23 H23A 109.4 . .
N4 C23 H23B 109.4 . .
H23A C23 H23B 108.0 . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C32 C35 H35A 109.5 . .
C32 C35 H35B 109.5 . .
C32 C35 H35C 109.5 . .
H35A C35 H35B 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C32 C34 H34A 109.5 . .
C32 C34 H34B 109.5 . .
C32 C34 H34C 109.5 . .
H34A C34 H34B 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C28 C30 H30A 109.5 . .
C28 C30 H30B 109.5 . .
C28 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C28 C31 H31A 109.5 . .
C28 C31 H31B 109.5 . .
C28 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N5 C36 C37 177.6(17) . .
C36 C37 H37A 109.5 . .
C36 C37 H37B 109.5 . .
C36 C37 H37C 109.5 . .
H37A C37 H37B 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 N1 2.405(3) 5
Lu1 N1 2.405(3) .
Lu1 N1 2.405(3) 9
Lu1 O1 2.148(3) 5
Lu1 O1 2.148(3) 9
Lu1 O1 2.148(3) .
Lu1 N4 2.680(6) .
C1 C2 1.419(5) .
C1 O1 1.307(4) .
C1 C6 1.431(5) .
N1 C7 1.280(5) .
N1 C22 1.465(5) .
C2 C7 1.435(5) .
C2 C3 1.409(5) .
C6 C32 1.529(5) .
C6 C5 1.383(5) .
C7 H7 0.9500 .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C22 C23 1.509(6) .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C33 C32 1.532(5) .
C28 C4 1.525(5) .
C28 C29 1.534(6) .
C28 C30 1.534(6) .
C28 C31 1.541(6) .
N4 C23 1.484(4) 9
N4 C23 1.484(4) 5
N4 C23 1.484(4) .
C32 C35 1.538(6) .
C32 C34 1.536(6) .
C4 C3 1.371(6) .
C4 C5 1.412(5) .
C3 H3 0.9500 .
C5 H5 0.9500 .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C36 C37 1.431(14) .
C36 N5 1.094(14) .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23A N5 0.99 2.62 3.477(13) 145.1 .
