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_1572903
_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 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     dual
_audit_creation_date             2023-08-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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                   11.983(2)
_cell_length_b                   12.877(3)
_cell_length_c                   8.8927(17)
_cell_measurement_reflns_used    1028
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      18.337
_cell_measurement_theta_min      2.853
_cell_volume                     1372.2(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1352
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15587
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.146
_diffrn_reflns_theta_min         2.784
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0742 after correction.
The Ratio of minimum to maximum transmission is 0.8046.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.891
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1435
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0372P)^2^+0.5586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                855
_reflns_number_total             1435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04767b3.cif
_cod_data_source_block           2-Nd-trans
_cod_depositor_comments
'Adding full bibliography for 1572887--1572904.cif.'
_cod_database_code               1572903
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.520
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4B-C5B \\sim C5B_$1-C5B \\sim C4B_$1-C5B_$1 \\sim C4B_$1-C3B_$1 \\sim
C3B_$1-C2B_$1 \\sim C2B_$1-
 C1B \\sim C2B-C1B \\sim C3B-C2B \\sim C4B-C3B
 with sigma of 0.02
 C1A-C2A_$1 \\sim C1A-C2A \\sim C3A-C2A \\sim C3A-C4A \\sim C4A-C5A \\sim
C5A-C5A_$1 \\sim C4A_$1-
 C5A_$1 \\sim C3A_$1-C4A_$1 \\sim C3A_$1-C2A_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C5B \\sim C2A \\sim C4B \\sim C3A \\sim C3B \\sim C4A \\sim C2B \\sim
C5A \\sim C1B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
4. Others
 Sof(C2B)=Sof(H2B)=Sof(C5B)=Sof(H5B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=1-
 FVAR(1)
 Sof(C1B)=Sof(H1B)=0.5*(1-FVAR(2))
 Sof(C1A)=Sof(H1A)=0.5*FVAR(2)
 Sof(C5A)=Sof(H5A)=Sof(C2A)=Sof(H2A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C5A(H5A), C2A(H2A), C4A(H4A), C7(H7), C8(H8), C3A(H3A),
 C1A(H1A), C1B(H1B), C2B(H2B), C5B(H5B), C3B(H3B), C4B(H4B)
;
_shelx_res_checksum              69464
_olex2_submission_special_instructions 'No special instructions were received'