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#$Date: 2019-11-07 23:01:00 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223914 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/06/7700642.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_7700642
loop_
_publ_author_name
'Long, Jérôme'
'Skvortsov, Grigorii G.'
'Cherkasov, Anton V.'
'Lyssenko, Konstantin A.'
'Poddel'sky, Andrei I.'
'Guari, Yannick'
'Larionova, Joulia'
'Trifonov, Alexander A.'
_publ_section_title
;
 Synthesis, structure and magnetic properties of a series of Ln(iii)
 complexes with radical-anionic iminopyridine ligands: effect of
 lanthanide ions on the slow relaxation of the magnetization.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12018
_journal_page_last               12022
_journal_paper_doi               10.1039/c9dt00738e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C54 H66 Er N6, 0.5(C7 H8)'
_chemical_formula_sum            'C57.5 H70 Er N6'
_chemical_formula_weight         1012.45
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-12-06 deposited with the CCDC.    2019-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.5889(3)
_cell_length_b                   18.5889(3)
_cell_length_c                   25.4010(7)
_cell_measurement_reflns_used    18370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7820
_cell_measurement_theta_min      3.4260
_cell_volume                     7601.3(3)
_computing_cell_refinement       'CrysAlis Pro'
_computing_data_collection       'CrysAlis Pro'
_computing_data_reduction        'CrysAlis Pro'
_computing_structure_refinement  'SHELXL 2017/1'
_computing_structure_solution    'SHELXT 2014/5'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur EOS (CCD)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35624
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.094
_diffrn_reflns_theta_min         2.996
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis Pro 1.171.38.46. Numerical absorption correction based on gaussian
integration over a multifaceted crystal model. Empirical absorption correction
using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       prism
_exptl_crystal_F_000             3150
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0325P)²+12.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3266
_reflns_number_total             3725
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00738e2.cif
_cod_data_source_block           erimmepy
_cod_depositor_comments
'Adding full bibliography for 7700641--7700645.cif.'
_cod_original_formula_sum        'C57.50 H70 Er N6'
_cod_database_code               7700642
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.630
_shelx_estimated_absorpt_t_max   0.738
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Er1 Er 0.666667 0.333333 0.49631(2) 0.03459(7) Uani 1 3 d S T P . .
N1 N 0.67013(10) 0.43593(10) 0.43768(8) 0.0369(4) Uani 1 1 d . . . . .
N2 N 0.57190(10) 0.37514(10) 0.52567(9) 0.0399(4) Uani 1 1 d . . . . .
C1 C 0.72148(13) 0.47175(12) 0.39637(10) 0.0420(5) Uani 1 1 d . . . . .
H1A H 0.758485 0.452382 0.387389 0.050 Uiso 1 1 calc R U . . .
C2 C 0.72372(15) 0.53401(14) 0.36661(11) 0.0485(6) Uani 1 1 d . . . . .
H2A H 0.761746 0.557475 0.338198 0.058 Uiso 1 1 calc R U . . .
C3 C 0.66844(16) 0.56276(14) 0.37893(12) 0.0527(6) Uani 1 1 d . . . . .
H3A H 0.668632 0.606071 0.358958 0.063 Uiso 1 1 calc R U . . .
C4 C 0.61514(15) 0.52769(13) 0.41962(11) 0.0478(6) Uani 1 1 d . . . . .
H4A H 0.576791 0.545686 0.427882 0.057 Uiso 1 1 calc R U . . .
C5 C 0.61614(12) 0.46435(12) 0.44998(10) 0.0397(5) Uani 1 1 d . . . . .
C6 C 0.56540(12) 0.42910(12) 0.49399(11) 0.0417(5) Uani 1 1 d . . . . .
H6A H 0.524589 0.444061 0.501740 0.050 Uiso 1 1 calc R U . . .
C7 C 0.51184(8) 0.34398(9) 0.56766(7) 0.0468(6) Uani 1 1 d G . . . .
C8 C 0.53592(8) 0.37616(10) 0.61810(7) 0.0595(7) Uani 1 1 d G . . . .
C9 C 0.47851(13) 0.34666(14) 0.65897(6) 0.0764(10) Uani 1 1 d G . . . .
H9A H 0.494965 0.368654 0.693443 0.092 Uiso 1 1 calc R U . . .
C10 C 0.39701(12) 0.28496(13) 0.64940(8) 0.0889(13) Uani 1 1 d G . . . .
H10A H 0.357765 0.264797 0.677325 0.107 Uiso 1 1 calc R U . . .
C11 C 0.37292(8) 0.25278(10) 0.59896(10) 0.0790(12) Uani 1 1 d G . . . .
H11A H 0.317223 0.210613 0.592412 0.095 Uiso 1 1 calc R U . . .
C12 C 0.43034(9) 0.28228(9) 0.55809(7) 0.0576(8) Uani 1 1 d G . . . .
C13 C 0.62325(18) 0.4478(2) 0.62875(14) 0.0727(9) Uani 1 1 d . . . . .
H13A H 0.662192 0.439032 0.606108 0.087 Uiso 1 1 calc R U . . .
C14 C 0.6306(2) 0.5299(2) 0.6123(2) 0.1083(15) Uani 1 1 d . . . . .
H14A H 0.617562 0.527942 0.574708 0.163 Uiso 1 1 calc R U . . .
H14B H 0.687360 0.575203 0.618648 0.163 Uiso 1 1 calc R U . . .
H14C H 0.591524 0.539547 0.632780 0.163 Uiso 1 1 calc R U . . .
C15 C 0.6524(3) 0.4538(4) 0.68575(19) 0.1212(18) Uani 1 1 d . . . . .
H15A H 0.645618 0.400179 0.696665 0.182 Uiso 1 1 calc R U . . .
H15B H 0.619149 0.468286 0.708687 0.182 Uiso 1 1 calc R U . . .
H15C H 0.711060 0.496712 0.688397 0.182 Uiso 1 1 calc R U . . .
C16 C 0.40008(14) 0.24745(15) 0.50309(15) 0.0660(9) Uani 1 1 d . . . . .
H16A H 0.450129 0.267326 0.480074 0.079 Uiso 1 1 calc R U . . .
C17 C 0.3455(2) 0.2794(2) 0.47937(18) 0.0869(12) Uani 1 1 d . . . . .
H17A H 0.330943 0.259387 0.443079 0.130 Uiso 1 1 calc R U . . .
H17B H 0.375898 0.340245 0.479579 0.130 Uiso 1 1 calc R U . . .
H17C H 0.294633 0.258894 0.500286 0.130 Uiso 1 1 calc R U . . .
C18 C 0.35273(18) 0.15226(17) 0.50141(18) 0.0812(10) Uani 1 1 d . U . . .
H18A H 0.337896 0.133541 0.464915 0.122 Uiso 1 1 calc R U . . .
H18B H 0.302090 0.130887 0.522619 0.122 Uiso 1 1 calc R U . . .
H18C H 0.387949 0.131494 0.515616 0.122 Uiso 1 1 calc R U . . .
C1S C 0.6443(16) 0.3638(19) 0.8239(15) 0.180(11) Uani 0.1667 1 d DG U P A -1
H1SA H 0.598515 0.372907 0.826880 0.215 Uiso 0.1667 1 calc R U P A -1
C2S C 0.7202(19) 0.4266(18) 0.8052(13) 0.173(11) Uani 0.1667 1 d G U P A -1
H2SA H 0.726286 0.478715 0.795449 0.208 Uiso 0.1667 1 calc R U P A -1
C3S C 0.7871(13) 0.413(2) 0.8009(9) 0.166(11) Uani 0.1667 1 d G U P A -1
H3SA H 0.838975 0.456184 0.788106 0.199 Uiso 0.1667 1 calc R U P A -1
C4S C 0.7781(13) 0.337(2) 0.8152(11) 0.127(8) Uani 0.1667 1 d G U P A -1
H4SA H 0.823894 0.327846 0.812194 0.152 Uiso 0.1667 1 calc R U P A -1
C5S C 0.7022(15) 0.2741(19) 0.8338(12) 0.142(10) Uani 0.1667 1 d DG U P A -1
H5SA H 0.696123 0.222037 0.843625 0.170 Uiso 0.1667 1 calc R U P A -1
C6S C 0.6353(11) 0.2875(16) 0.8382(12) 0.158(10) Uani 0.1667 1 d DG U P A -1
C7S C 0.5521(14) 0.2186(19) 0.8587(16) 0.145(10) Uani 0.1667 1 d D U P A -1
H7SA H 0.526481 0.242711 0.880913 0.217 Uiso 0.1667 1 calc R U P A -1
H7SB H 0.560934 0.179209 0.879425 0.217 Uiso 0.1667 1 calc R U P A -1
H7SC H 0.515466 0.189565 0.828902 0.217 Uiso 0.1667 1 calc R U P 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'
Er Er -0.2586 4.9576 '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
N2 Er1 N2 110.60(5) 2_655 3_665
N2 Er1 N2 110.60(5) 2_655 .
N2 Er1 N2 110.60(5) 3_665 .
N2 Er1 N1 155.68(7) 2_655 .
N2 Er1 N1 90.66(6) 3_665 .
N2 Er1 N1 70.34(6) . .
N2 Er1 N1 70.34(6) 2_655 2_655
N2 Er1 N1 155.68(7) 3_665 2_655
N2 Er1 N1 90.66(6) . 2_655
N1 Er1 N1 85.42(7) . 2_655
N2 Er1 N1 90.66(6) 2_655 3_665
N2 Er1 N1 70.34(6) 3_665 3_665
N2 Er1 N1 155.68(7) . 3_665
N1 Er1 N1 85.42(7) . 3_665
N1 Er1 N1 85.42(7) 2_655 3_665
C1 N1 C5 117.16(18) . .
C1 N1 Er1 127.40(13) . .
C5 N1 Er1 115.33(15) . .
C6 N2 C7 113.88(16) . .
C6 N2 Er1 114.62(14) . .
C7 N2 Er1 130.87(12) . .
N1 C1 C2 124.3(2) . .
N1 C1 H1A 117.9 . .
C2 C1 H1A 117.9 . .
C1 C2 C3 118.6(2) . .
C1 C2 H2A 120.7 . .
C3 C2 H2A 120.7 . .
C4 C3 C2 118.9(2) . .
C4 C3 H3A 120.5 . .
C2 C3 H3A 120.5 . .
C3 C4 C5 120.4(2) . .
C3 C4 H4A 119.8 . .
C5 C4 H4A 119.8 . .
N1 C5 C6 116.77(19) . .
N1 C5 C4 120.6(2) . .
C6 C5 C4 122.66(19) . .
N2 C6 C5 122.70(18) . .
N2 C6 H6A 118.7 . .
C5 C6 H6A 118.7 . .
C8 C7 C12 120.0 . .
C8 C7 N2 119.45(14) . .
C12 C7 N2 120.55(13) . .
C9 C8 C7 120.0 . .
C9 C8 C13 119.00(17) . .
C7 C8 C13 120.87(17) . .
C8 C9 C10 120.0 . .
C8 C9 H9A 120.0 . .
C10 C9 H9A 120.0 . .
C11 C10 C9 120.0 . .
C11 C10 H10A 120.0 . .
C9 C10 H10A 120.0 . .
C10 C11 C12 120.0 . .
C10 C11 H11A 120.0 . .
C12 C11 H11A 120.0 . .
C11 C12 C7 120.0 . .
C11 C12 C16 118.00(14) . .
C7 C12 C16 121.96(14) . .
C14 C13 C8 110.5(3) . .
C14 C13 C15 109.7(3) . .
C8 C13 C15 114.5(3) . .
C14 C13 H13A 107.3 . .
C8 C13 H13A 107.3 . .
C15 C13 H13A 107.3 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C12 C16 C17 111.8(2) . .
C12 C16 C18 113.1(3) . .
C17 C16 C18 109.1(2) . .
C12 C16 H16A 107.5 . .
C17 C16 H16A 107.5 . .
C18 C16 H16A 107.5 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C2S C1S C6S 120.0 . .
C2S C1S H1SA 120.0 . .
C6S C1S H1SA 120.0 . .
C1S C2S C3S 120.0 . .
C1S C2S H2SA 120.0 . .
C3S C2S H2SA 120.0 . .
C2S C3S C4S 120.0 . .
C2S C3S H3SA 120.0 . .
C4S C3S H3SA 120.0 . .
C5S C4S C3S 120.0 . .
C5S C4S H4SA 120.0 . .
C3S C4S H4SA 120.0 . .
C4S C5S C6S 120.0 . .
C4S C5S H5SA 120.0 . .
C6S C5S H5SA 120.0 . .
C5S C6S C1S 120.0 . .
C5S C6S C7S 120.0(4) . .
C1S C6S C7S 120.0(4) . .
C6S C7S H7SA 109.5 . .
C6S C7S H7SB 109.5 . .
H7SA C7S H7SB 109.5 . .
C6S C7S H7SC 109.5 . .
H7SA C7S H7SC 109.5 . .
H7SB C7S H7SC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Er1 N2 2.3733(16) 2_655
Er1 N2 2.3733(16) 3_665
Er1 N2 2.3733(16) .
Er1 N1 2.3950(18) .
Er1 N1 2.3950(18) 2_655
Er1 N1 2.3951(18) 3_665
N1 C1 1.349(3) .
N1 C5 1.384(2) .
N2 C6 1.338(3) .
N2 C7 1.440(2) .
C1 C2 1.365(3) .
C1 H1A 0.9500 .
C2 C3 1.410(3) .
C2 H2A 0.9500 .
C3 C4 1.353(4) .
C3 H3A 0.9500 .
C4 C5 1.415(3) .
C4 H4A 0.9500 .
C5 C6 1.396(3) .
C6 H6A 0.9500 .
C7 C8 1.3900 .
C7 C12 1.3900 .
C8 C9 1.3900 .
C8 C13 1.523(3) .
C9 C10 1.3900 .
C9 H9A 0.9500 .
C10 C11 1.3900 .
C10 H10A 0.9500 .
C11 C12 1.3900 .
C11 H11A 0.9500 .
C12 C16 1.524(4) .
C13 C14 1.522(6) .
C13 C15 1.530(6) .
C13 H13A 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.532(4) .
C16 C18 1.533(3) .
C16 H16A 1.0000 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C1S C2S 1.3900 .
C1S C6S 1.3900 .
C1S H1SA 0.9500 .
C2S C3S 1.3900 .
C2S H2SA 0.9500 .
C3S C4S 1.3900 .
C3S H3SA 0.9500 .
C4S C5S 1.3900 .
C4S H4SA 0.9500 .
C5S C6S 1.3900 .
C5S H5SA 0.9500 .
C6S C7S 1.524(10) .
C7S H7SA 0.9800 .
C7S H7SB 0.9800 .
C7S H7SC 0.9800 .
