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_1572901
_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         '3.204(C5.305 H5.305), Nd'
_chemical_formula_sum            'C17 H17 Nd'
_chemical_formula_weight         365.54
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_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                   12.0748(18)
_cell_length_b                   12.8129(19)
_cell_length_c                   8.8427(14)
_cell_measurement_reflns_used    1474
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      21.855
_cell_measurement_theta_min      2.855
_cell_volume                     1368.1(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1464
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28912
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.673
_diffrn_reflns_theta_min         2.799
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.773
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1009 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.8353.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1986
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0460P)^2^+0.8743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1036
_reflns_number_total             1986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04767b3.cif
_cod_data_source_block           2-Nd-cis
_cod_depositor_comments
'Adding full bibliography for 1572887--1572904.cif.'
_cod_database_code               1572901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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: 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
C6A \\sim C7A \\sim C8A \\sim C9A: 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 C9B \\sim C10B: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008 within 2A
4. Others
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=1-
 FVAR(1)
 Sof(C1B)=Sof(H1B)=0.5*(1-FVAR(2))
 Sof(C1A)=Sof(H1A)=0.5*FVAR(2)
 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)
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), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B),
 C10B(H10B), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A)
;
_shelx_res_checksum              76202
_olex2_submission_special_instructions 'No special instructions were received'