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_1572891
_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 Y'
_chemical_formula_sum            'C17 H17 Y'
_chemical_formula_weight         310.21
_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             2024-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 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                 101.791(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0169(6)
_cell_length_b                   8.7585(8)
_cell_length_c                   11.1560(9)
_cell_measurement_reflns_used    11340
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.97
_cell_volume                     671.15(10)
_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 X-Red 2.3.0.0 (STOE, 2021)
;
_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    '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 0.994
_diffrn_measurement_details
;
 1414 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  0.0446
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6569
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.981
_diffrn_source                   Axo_Mo
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.645
_exptl_absorpt_correction_T_max  0.5377
_exptl_absorpt_correction_T_min  0.1133
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.297
_refine_diff_density_min         -4.351
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1534
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.1254
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+46.9600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2668
_refine_ls_wR_factor_ref         0.2712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1314
_reflns_number_total             1534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04767b3.cif
_cod_data_source_block           2-Y-cis
_cod_depositor_comments
'Adding full bibliography for 1572887--1572904.cif.'
_cod_database_code               1572891
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C12-C11 \\sim C12-C13 \\sim C14-C13 \\sim C14-C15 \\sim C16-C15 \\sim C17-C16
\\sim C17-C9 \\sim C9-C10 ~
 C11-C10
 with sigma of 0.02
 C5-C4 \\sim C5-C6 \\sim C7-C6 \\sim C8-C7 \\sim C1-C8 \\sim C2-C1 \\sim C3-C2
\\sim C4-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C10 \\sim C9 \\sim C15 \\sim C16 \\sim C12 \\sim C11 \\sim
C17: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within
2A
C5 \\sim C4 \\sim C6 \\sim C1 \\sim C7 \\sim C2 \\sim C8 \\sim C3: within 2A
with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C10(H10), C9(H9), C15(H15), C16(H16), C12(H12), C11(H11),
 C17(H17), C5(H5), C4(H4), C6(H6), C1(H1), C7(H7), C2(H2), C8(H8), C3(H3)
;
_shelx_res_checksum              1253
_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   10.0
_stoe_evaluation_integration_b   2.5
_stoe_evaluation_integration_ems 0.024
_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 93.0
_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 57.7
_stoe_evaluation_lana_max_2theta_desired 57.7
_stoe_evaluation_lana_mean_redundancy 4.1
_stoe_evaluation_lana_number_refls_after_or 6711
_stoe_evaluation_lana_number_refls_outliers 926
_stoe_evaluation_lana_number_refls_total 7637
_stoe_evaluation_lana_number_refls_unique 1635
_stoe_evaluation_lana_number_refls_written 6711
_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           7.2   13.2   19.2   25.2   31.2   37.2   43.2   49.2   55.2
<Resolution>    5.04   2.97   2.11   1.61   1.32   1.11   0.96   0.85   0.78
N(total)         108    354    397    706   1030   1377   1447   1532    686
<Redundancy>     7.7    8.8    5.1    5.0    5.0    4.9    4.3    3.6    2.2
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0   99.7  100.0   70.9
<I/sigma>      322.1  140.4  103.9   39.9   24.0   15.2    6.2    4.2    2.6
R(int)         0.020  0.036  0.032  0.044  0.045  0.056  0.106  0.132  0.176
;
_stoe_measurement_identifier     LP197
_stoe_measurement_max_exposure_per_frame '180.0 s'
_stoe_measurement_mean_exposure_per_frame '180.0 s'
_stoe_measurement_min_exposure_per_frame '180.0 s'
_stoe_measurement_total_exposure_time '70.7 h'
_stoe_measurement_total_frame_number 1414
_stoe_measurement_total_run_number 13
_stoe_measurement_tube_power     '50.0 W'