The photo-isomerization of the cyclononatetraenyl ligand and related rare earth complexes.
Pedussaut, Lucie; Mahieu, Nolwenn; Chartier, Camille; Rajeshkumar, Thayalan; Tricoire, Maxime; Douair, Iskander; Casaretto, Nicolas; Maron, Laurent; Danoun, Grégory; Nocton, Grégory; Chemical science 15 (2024) 19273–19282; doi:10.1039/d4sc04767b

data_1572887
_publ_section_title
;
 The photo-isomerization of the cyclononatetraenyl ligand and related rare
 earth complexes.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              19273
_journal_page_last               19282
_journal_paper_doi               10.1039/d4sc04767b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C18 H18 Sm'
_chemical_formula_sum            'C18 H18 Sm'
_chemical_formula_weight         384.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-13 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.630(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3830(16)
_cell_length_b                   9.1133(11)
_cell_length_c                   11.059(2)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.91
_cell_volume                     735.7(2)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      '1033 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1487
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.004
_diffrn_reflns_theta_min         2.910
_diffrn_source                   Axo_Mo
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.974
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.055
_refine_diff_density_max         5.142
_refine_diff_density_min         -2.660
_refine_diff_density_rms         0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1448
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0959
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2434
_refine_ls_wR_factor_ref         0.2613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                885
_reflns_number_total             1448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04767b3.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1572887--1572904.cif.'
_cod_original_cell_volume        735.6(2)
_cod_database_code               1572887
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{C2A, C2B}
{C3A, C3B}
{C4A, C4B}
{C5A, C5B}
{C6A, C6B}
{C7A, C7B}
{C8A, C8B}
{C9A, C9B}
3. Restrained distances
 C1A-C2A \\sim C2A-C3A \\sim C3A-C4A \\sim C4A-C5A \\sim C5A-C6A \\sim C6A-C7A
\\sim C7A-C8A \\sim C8A-C9A
 \\sim C9A-C1A
 with sigma of 0.02
 C1B-C2B \\sim C2B-C3B \\sim C3B-C4B \\sim C4B-C5B \\sim C5B-C6B \\sim C6B-C7B
\\sim C7B-C8B \\sim C8B-C9B
 \\sim C9B-C1B
 with sigma of 0.02
 C1C-C2C \\sim C2C-C3C \\sim C3C-C4C \\sim C4C-C5C \\sim C5C-C6C \\sim C6C-C7C
\\sim C7C-C8C \\sim C8C-C9C
 \\sim C9C-C1C
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C2A \\sim C2B \\sim C2C \\sim C3A \\sim C3B \\sim
C3C \\sim C4A \\sim C4B \\sim C4C \\sim C5A \\sim C5B \\sim C5C \\sim C6A \\sim
C6B \\sim C6C \\sim C7A \\sim C7B \\sim C7C \\sim C8A \\sim C8B \\sim C8C \\sim
C9A \\sim C9B \\sim C9C: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(C6A) = Uanis(C6B)
Uanis(C5A) = Uanis(C5B)
Uanis(C7A) = Uanis(C7B)
Uanis(C8A) = Uanis(C8B)
Uanis(C9A) = Uanis(C9B)
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C2A, C2B, C2C, C3A, C3B, C3C, C4A, C4B, C4C, C5A, C5B, C5C,
 C6A, C6B, C6C, C7A, C7B, C7C, C8A, C8B, C8C, C9A, C9B, C9C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(C1A)+Sof(H1A)+Sof(C2A)+Sof(H2A)+Sof(C3A)+Sof(H3A)+Sof(C4A)+Sof(H4A)+
 Sof(C5A)+Sof(H5A)+Sof(C6A)+Sof(H6A)+Sof(C7A)+Sof(H7A)+Sof(C8A)+Sof(H8A)+
 Sof(C9A)+Sof(H9A)]+1*[Sof(C1B)+Sof(H1B)+Sof(C2B)+Sof(H2B)+Sof(C3B)+Sof(H3B)+
 Sof(C4B)+Sof(H4B)+Sof(C5B)+Sof(H5B)+Sof(C6B)+Sof(H6B)+Sof(C7B)+Sof(H7B)+
 Sof(C8B)+Sof(H8B)+Sof(C9B)+Sof(H9B)]+1*[Sof(C1C)+Sof(H1C)+Sof(C2C)+Sof(H2C)+
 Sof(C3C)+Sof(H3C)+Sof(C4C)+Sof(H4C)+Sof(C5C)+Sof(H5C)+Sof(C6C)+Sof(H6C)+
 Sof(C7C)+Sof(H7C)+Sof(C8C)+Sof(H8C)+Sof(C9C)+Sof(H9C)]=1 with esd of 0.00001
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=
 Sof(C9A)=Sof(H9A)=FVAR(1)
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=
 Sof(C9B)=Sof(H9B)=FVAR(2)
 Sof(C1C)=Sof(H1C)=Sof(C2C)=Sof(H2C)=Sof(C3C)=Sof(H3C)=Sof(C4C)=Sof(H4C)=
 Sof(C5C)=Sof(H5C)=Sof(C6C)=Sof(H6C)=Sof(C7C)=Sof(H7C)=Sof(C8C)=Sof(H8C)=
 Sof(C9C)=Sof(H9C)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C1C(H1C), C2A(H2A), C2B(H2B), C2C(H2C), C3A(H3A),
 C3B(H3B), C3C(H3C), C4A(H4A), C4B(H4B), C4C(H4C), C5A(H5A), C5B(H5B), C5C(H5C),
  C6A(H6A), C6B(H6B), C6C(H6C), C7A(H7A), C7B(H7B), C7C(H7C), C8A(H8A),
 C8B(H8B), C8C(H8C), C9A(H9A), C9B(H9B), C9C(H9C)
;
_shelx_res_checksum              98254
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   14.5
_stoe_evaluation_integration_b   0.7
_stoe_evaluation_integration_ems 0.013
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 93.4
_stoe_evaluation_lana_dxs_max_order 3
_stoe_evaluation_lana_dys_max_order 3
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 58.5
_stoe_evaluation_lana_max_2theta_desired 58.5
_stoe_evaluation_lana_mean_redundancy 6.0
_stoe_evaluation_lana_number_refls_after_or 11825
_stoe_evaluation_lana_number_refls_outliers 1397
_stoe_evaluation_lana_number_refls_total 13222
_stoe_evaluation_lana_number_refls_unique 1984
_stoe_evaluation_lana_number_refls_written 11825
_stoe_evaluation_lana_or_c1      0.050
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      1.0
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           6.6   12.8   19.0   25.2   31.4   37.6   43.8   50.0   56.2
<Resolution>    5.27   3.10   2.17   1.60   1.31   1.10   0.95   0.84   0.77
N(total)         179    588    709   1110   1746   2247   2720   2871   1052
<Redundancy>    11.8   11.4    7.6    6.8    7.3    7.0    6.4    5.5    2.9
Complet. [%%]   100.0  100.0   98.8  100.0  100.0  100.0  100.0  100.0   71.4
<I/sigma>      141.6   53.6   61.9   25.2   15.1    7.7    4.0    2.1    1.7
R(int)         0.078  0.078  0.127  0.151  0.187  0.197  0.227  0.269  0.970
;
_stoe_measurement_identifier     LP227
_stoe_measurement_max_exposure_per_frame '75.0 s'
_stoe_measurement_mean_exposure_per_frame '75.0 s'
_stoe_measurement_min_exposure_per_frame '75.0 s'
_stoe_measurement_total_exposure_time '21.5 h'
_stoe_measurement_total_frame_number 1033
_stoe_measurement_total_run_number 17
_stoe_measurement_tube_power     '50.0 W'