#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:01:00 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223914 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/06/7700645.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_7700645
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 Gd N6, 0.5(C7 H8)'
_chemical_formula_sum            'C57.5 H70 Gd N6'
_chemical_formula_weight         1002.44
_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
;
2019-06-17 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                   18.6764(14)
_cell_length_b                   18.6764(14)
_cell_length_c                   25.337(2)
_cell_measurement_reflns_used    9516
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.18
_cell_volume                     7653.7(10)
_computing_cell_refinement       'Saint 8.37a'
_computing_data_collection       'APEX3 2016.9'
_computing_data_reduction        'Saint 8.37a'
_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 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35561
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.718
_diffrn_reflns_theta_min         2.412
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       plate
_exptl_crystal_F_000             3126
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0317P)²+21.8990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3957
_reflns_number_total             4396
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00738e2.cif
_cod_data_source_block           gdimmepy
_cod_depositor_comments
'Adding full bibliography for 7700641--7700645.cif.'
_cod_original_cell_volume        7653.7(13)
_cod_original_formula_sum        'C57.50 H70 Gd N6'
_cod_database_code               7700645
_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   0.824
_shelx_estimated_absorpt_t_max   0.936
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
Gd1 Gd 0.666667 0.333333 0.49827(2) 0.03273(7) Uani 1 3 d S T P . .
N1 N 0.66887(10) 0.43716(10) 0.43760(8) 0.0351(4) Uani 1 1 d . . . . .
N2 N 0.57035(10) 0.37687(10) 0.52555(9) 0.0372(4) Uani 1 1 d . . . . .
C1 C 0.72025(13) 0.47253(13) 0.39619(10) 0.0397(5) Uani 1 1 d . . . . .
H1A H 0.757152 0.453216 0.387473 0.048 Uiso 1 1 calc R U . . .
C2 C 0.72256(15) 0.53443(14) 0.36597(12) 0.0463(6) Uani 1 1 d . . . . .
H2A H 0.760630 0.557753 0.337596 0.056 Uiso 1 1 calc R U . . .
C3 C 0.66728(16) 0.56277(14) 0.37786(12) 0.0487(6) Uani 1 1 d . . . . .
H3A H 0.667584 0.605767 0.357659 0.058 Uiso 1 1 calc R U . . .
C4 C 0.61369(15) 0.52790(14) 0.41848(11) 0.0454(6) Uani 1 1 d . . . . .
H4A H 0.575238 0.545635 0.426310 0.054 Uiso 1 1 calc R U . . .
C5 C 0.61460(12) 0.46506(12) 0.44941(10) 0.0368(5) Uani 1 1 d . . . . .
C6 C 0.56347(12) 0.43022(12) 0.49324(11) 0.0394(5) Uani 1 1 d . . . . .
H6A H 0.522398 0.444696 0.500494 0.047 Uiso 1 1 calc R U . . .
C7 C 0.51093(8) 0.34549(9) 0.56784(7) 0.0442(6) Uani 1 1 d G . . . .
C8 C 0.53538(9) 0.37698(10) 0.61848(8) 0.0569(7) Uani 1 1 d G . . . .
C9 C 0.47877(13) 0.34676(14) 0.65973(6) 0.0741(10) Uani 1 1 d G . . . .
H9A H 0.495485 0.368282 0.694344 0.089 Uiso 1 1 calc R U . . .
C10 C 0.39771(12) 0.28505(13) 0.65035(8) 0.0861(14) Uani 1 1 d G . . . .
H10A H 0.359020 0.264394 0.678541 0.103 Uiso 1 1 calc R U . . .
C11 C 0.37326(8) 0.25356(10) 0.59971(10) 0.0754(12) Uani 1 1 d G . . . .
H11A H 0.317853 0.211382 0.593293 0.090 Uiso 1 1 calc R U . . .
C12 C 0.42986(9) 0.28378(9) 0.55846(7) 0.0551(8) Uani 1 1 d G . . . .
C13 C 0.62230(19) 0.4482(2) 0.62896(15) 0.0717(9) Uani 1 1 d . . . . .
H13A H 0.660909 0.439426 0.606098 0.086 Uiso 1 1 calc R U . . .
C14 C 0.6300(3) 0.5302(2) 0.6130(2) 0.1076(17) Uani 1 1 d . . . . .
H14A H 0.613674 0.527504 0.575982 0.161 Uiso 1 1 calc R U . . .
H14B H 0.687446 0.574496 0.617409 0.161 Uiso 1 1 calc R U . . .
H14C H 0.593893 0.541385 0.635337 0.161 Uiso 1 1 calc R U . . .
C15 C 0.6521(3) 0.4547(4) 0.6862(2) 0.1210(19) Uani 1 1 d . . . . .
H15A H 0.645895 0.401574 0.697209 0.182 Uiso 1 1 calc R U . . .
H15B H 0.619010 0.468938 0.709334 0.182 Uiso 1 1 calc R U . . .
H15C H 0.710411 0.497740 0.688599 0.182 Uiso 1 1 calc R U . . .
C16 C 0.39924(15) 0.24919(15) 0.50299(15) 0.0630(9) Uani 1 1 d . . . . .
H16A H 0.448829 0.270503 0.479558 0.076 Uiso 1 1 calc R U . . .
C17 C 0.3427(2) 0.2790(2) 0.48011(19) 0.0846(12) Uani 1 1 d . . . . .
H17A H 0.326560 0.257863 0.444097 0.127 Uiso 1 1 calc R U . . .
H17B H 0.372173 0.339612 0.479507 0.127 Uiso 1 1 calc R U . . .
H17C H 0.293082 0.258701 0.502104 0.127 Uiso 1 1 calc R U . . .
C18 C 0.35477(19) 0.15459(17) 0.50106(18) 0.0790(10) Uani 1 1 d . U . . .
H18A H 0.338999 0.135939 0.464570 0.118 Uiso 1 1 calc R U . . .
H18B H 0.305098 0.131742 0.523159 0.118 Uiso 1 1 calc R U . . .
H18C H 0.391775 0.135575 0.514224 0.118 Uiso 1 1 calc R U . . .
C1S C 0.6453(14) 0.3637(17) 0.8148(10) 0.183(11) Uani 0.1667 1 d DG U P A -1
H1SA H 0.598430 0.370949 0.815797 0.219 Uiso 0.1667 1 calc R U P A -1
C2S C 0.7205(17) 0.4269(16) 0.7962(10) 0.164(10) Uani 0.1667 1 d G U P A -1
H2SA H 0.725117 0.477316 0.784439 0.197 Uiso 0.1667 1 calc R U P A -1
C3S C 0.7890(13) 0.4162(17) 0.7947(7) 0.154(10) Uani 0.1667 1 d G U P A -1
H3SA H 0.840451 0.459417 0.781984 0.184 Uiso 0.1667 1 calc R U P A -1
C4S C 0.7823(11) 0.3424(19) 0.8119(9) 0.100(7) Uani 0.1667 1 d G U P A -1
H4SA H 0.829099 0.335149 0.810886 0.120 Uiso 0.1667 1 calc R U P A -1
C5S C 0.7070(13) 0.2792(15) 0.8305(10) 0.123(8) Uani 0.1667 1 d DG U P A -1
H5SA H 0.702413 0.228781 0.842243 0.147 Uiso 0.1667 1 calc R U P A -1
C6S C 0.6385(10) 0.2899(14) 0.8320(9) 0.148(10) Uani 0.1667 1 d DG U P A -1
C7S C 0.5559(12) 0.2206(17) 0.8525(13) 0.114(8) Uani 0.1667 1 d D U P A -1
H7SA H 0.521167 0.243675 0.863237 0.171 Uiso 0.1667 1 calc R U P A -1
H7SB H 0.565504 0.194002 0.882833 0.171 Uiso 0.1667 1 calc R U P A -1
H7SC H 0.527979 0.179677 0.824482 0.171 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'
Gd Gd -0.1653 3.9035 '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 Gd1 N2 112.17(5) 2_655 3_665
N2 Gd1 N2 112.17(5) 2_655 .
N2 Gd1 N2 112.16(5) 3_665 .
N2 Gd1 N1 90.35(6) 2_655 3_665
N2 Gd1 N1 68.60(6) 3_665 3_665
N2 Gd1 N1 153.55(6) . 3_665
N2 Gd1 N1 153.55(6) 2_655 .
N2 Gd1 N1 90.34(6) 3_665 .
N2 Gd1 N1 68.60(6) . .
N1 Gd1 N1 85.04(7) 3_665 .
N2 Gd1 N1 68.60(6) 2_655 2_655
N2 Gd1 N1 153.55(6) 3_665 2_655
N2 Gd1 N1 90.35(6) . 2_655
N1 Gd1 N1 85.05(7) 3_665 2_655
N1 Gd1 N1 85.05(7) . 2_655
C1 N1 C5 117.31(18) . .
C1 N1 Gd1 126.80(13) . .
C5 N1 Gd1 115.78(15) . .
C6 N2 C7 114.52(16) . .
C6 N2 Gd1 116.01(14) . .
C7 N2 Gd1 128.90(12) . .
N1 C1 C2 124.2(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 119.1(2) . .
C4 C3 H3A 120.4 . .
C2 C3 H3A 120.4 . .
C3 C4 C5 120.4(2) . .
C3 C4 H4A 119.8 . .
C5 C4 H4A 119.8 . .
N1 C5 C6 117.11(19) . .
N1 C5 C4 120.4(2) . .
C6 C5 C4 122.48(19) . .
N2 C6 C5 122.24(18) . .
N2 C6 H6A 118.9 . .
C5 C6 H6A 118.9 . .
C8 C7 C12 120.0 . .
C8 C7 N2 119.44(14) . .
C12 C7 N2 120.56(14) . .
C7 C8 C9 120.0 . .
C7 C8 C13 120.80(18) . .
C9 C8 C13 119.09(18) . .
C10 C9 C8 120.0 . .
C10 C9 H9A 120.0 . .
C8 C9 H9A 120.0 . .
C9 C10 C11 120.0 . .
C9 C10 H10A 120.0 . .
C11 C10 H10A 120.0 . .
C12 C11 C10 120.0 . .
C12 C11 H11A 120.0 . .
C10 C11 H11A 120.0 . .
C11 C12 C7 120.0 . .
C11 C12 C16 118.06(15) . .
C7 C12 C16 121.90(15) . .
C14 C13 C8 110.9(3) . .
C14 C13 C15 108.9(4) . .
C8 C13 C15 114.8(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 . .
C18 C16 C12 112.8(3) . .
C18 C16 C17 109.4(2) . .
C12 C16 C17 111.9(2) . .
C18 C16 H16A 107.5 . .
C12 C16 H16A 107.5 . .
C17 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 . .
C4S C3S C2S 120.0 . .
C4S C3S H3SA 120.0 . .
C2S C3S H3SA 120.0 . .
C3S C4S C5S 120.0 . .
C3S C4S H4SA 120.0 . .
C5S C4S H4SA 120.0 . .
C6S C5S C4S 120.0 . .
C6S C5S H5SA 120.0 . .
C4S C5S H5SA 120.0 . .
C5S C6S C1S 120.0 . .
C5S C6S C7S 120.1(4) . .
C1S C6S C7S 119.9(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
Gd1 N2 2.4160(17) 2_655
Gd1 N2 2.4160(17) 3_665
Gd1 N2 2.4160(16) .
Gd1 N1 2.4587(18) 3_665
Gd1 N1 2.4587(18) .
Gd1 N1 2.4587(18) 2_655
N1 C1 1.351(3) .
N1 C5 1.384(2) .
N2 C6 1.344(3) .
N2 C7 1.440(2) .
C1 C2 1.369(3) .
C1 H1A 0.9500 .
C2 C3 1.408(3) .
C2 H2A 0.9500 .
C3 C4 1.354(4) .
C3 H3A 0.9500 .
C4 C5 1.418(3) .
C4 H4A 0.9500 .
C5 C6 1.395(3) .
C6 H6A 0.9500 .
C7 C8 1.3900 .
C7 C12 1.3900 .
C8 C9 1.3900 .
C8 C13 1.521(4) .
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 1.533(4) .
C13 C14 1.520(6) .
C13 C15 1.536(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 C18 1.532(4) .
C16 C17 1.534(4) .
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 1.525(10) .
C7S H7SA 0.9800 .
C7S H7SB 0.9800 .
C7S H7SC 0.9800 .
