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_1572890
_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         'C17 H17 La'
_chemical_formula_sum            'C17 H17 La'
_chemical_formula_weight         360.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-13 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1385(7)
_cell_length_b                   12.7452(11)
_cell_length_c                   8.9543(11)
_cell_measurement_reflns_used    10162
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.78
_cell_volume                     1385.3(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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_details
;
 672 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  0.0335
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14590
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.340
_diffrn_reflns_theta_min         2.780
_diffrn_source                   Axo_Mo
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.062
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         1840
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1221
_reflns_number_total             1840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04767b3.cif
_cod_data_source_block           2-La-trans
_cod_depositor_comments
'Adding full bibliography for 1572887--1572904.cif.'
_cod_database_code               1572890
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1A-C2A \\sim C2A-C3A \\sim C3A-C4A \\sim C4A-C5A \\sim C5A-C5A_$1
 with sigma of 0.02
 C1B-C2B \\sim C2B-C3B \\sim C3B-C4B \\sim C4B-C5B \\sim C5B-C5B_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C1C: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
C6B \\sim C7B \\sim C8B \\sim C9B \\sim C10B: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
C6A \\sim C7A \\sim C8A \\sim C9A: within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 2A
4. Others
 1*[Sof(C1A)+Sof(H1A)]+1*[Sof(C1C)+Sof(H1C)]+1*[Sof(C1B)+Sof(H1B)]=1 with esd
 of 0.001
 1*[Sof(C2A)+Sof(H2A)+Sof(C3A)+Sof(H3A)+Sof(C4A)+Sof(H4A)+Sof(C5A)+Sof(H5A)]+1*
 [Sof(C2B)+Sof(H2B)+Sof(C3B)+Sof(H3B)+Sof(C4B)+Sof(H4B)+Sof(C5B)+Sof(H5B)]=1
 with esd of 0.0001
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=FVAR(1)
 Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=1-FVAR(2)
 Sof(C6B)=Sof(H6B)=Sof(C10B)=Sof(H10B)=0.5*(1-FVAR(3))
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=FVAR(2)
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=FVAR(3)
 Sof(C1A)=Sof(H1A)=0.5*FVAR(5)
 Sof(C1C)=Sof(H1C)=0.5*FVAR(6)
 Sof(C1B)=Sof(H1B)=0.5*FVAR(7)
5.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C1B(H1B), C2B(H2B),
 C3B(H3B), C4B(H4B), C5B(H5B), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A), C6B(H6B),
  C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B)
;
_shelx_res_checksum              7509
_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 6
_stoe_evaluation_lana_bos_l_odd_max 3
_stoe_evaluation_lana_completeness 92.6
_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 58.7
_stoe_evaluation_lana_max_2theta_desired 58.7
_stoe_evaluation_lana_mean_redundancy 7.9
_stoe_evaluation_lana_number_refls_after_or 14590
_stoe_evaluation_lana_number_refls_outliers 627
_stoe_evaluation_lana_number_refls_total 15217
_stoe_evaluation_lana_number_refls_unique 1840
_stoe_evaluation_lana_number_refls_written 14590
_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 mmm
_stoe_evaluation_lana_table
;
2Theta           6.8   13.0   19.2   25.4   31.6   37.8   44.0   50.2   56.4
<Resolution>    5.29   3.08   2.15   1.59   1.30   1.09   0.95   0.84   0.77
N(total)         185    654    826   1293   2036   2702   3127   3340   1054
<Redundancy>    14.3   15.9    9.5    8.9    9.7    9.7    8.6    7.4    3.3
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   68.1
<I/sigma>      151.4   54.8   56.0   28.8   20.3   11.5    8.2    5.1    2.9
R(int)         0.018  0.023  0.023  0.027  0.026  0.037  0.045  0.065  0.094
;
_stoe_measurement_identifier     LP175
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '10.0 s'
_stoe_measurement_min_exposure_per_frame '10.0 s'
_stoe_measurement_total_exposure_time '112 min'
_stoe_measurement_total_frame_number 672
_stoe_measurement_total_run_number 11
_stoe_measurement_tube_power     '50.0 W'