Electron transfer pathways in photoexcited lanthanide(iii) complexes of picolinate ligands.
Kovacs, Daniel; Kocsi, Daniel; Wells, Jordann A. L.; Kiraev, Salauat R.; Borbas, K. Eszter; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4244–4254; doi:10.1039/d1dt00616a

data_7706728
_publ_section_title
;
 Electron transfer pathways in photoexcited lanthanide(iii) complexes of
 picolinate ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4244
_journal_page_last               4254
_journal_paper_doi               10.1039/d1dt00616a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C35 H33 Cl0.5 F6 N7 O7.5 Tb, 0.5(Cl), 3(O), 0.5(H O)'
_chemical_formula_sum            'C35 H33.5 Cl F6 N7 O11 Tb'
_chemical_formula_weight         1036.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-21 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.661(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0772(4)
_cell_length_b                   22.4559(7)
_cell_length_c                   15.1582(5)
_cell_measurement_reflns_used    7612
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.543
_cell_measurement_theta_min      2.333
_cell_volume                     4077.2(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1209
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48003
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.700
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1653 before and 0.0681 after correction. The Ratio of minimum to maximum transmission is 0.8270. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       plate
_exptl_crystal_F_000             2066
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Glyme diffusion into aqueous solution'
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         6946
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0467P)^2^+11.3546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4901
_reflns_number_total             6946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00616a2.cif
_cod_data_source_block           eb2002
_cod_depositor_comments
'Adding full bibliography for 7706725--7706728.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C35 H33.50 Cl F6 N7 O11 Tb'
_cod_database_code               7706728
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.740
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5S-H5S
 0.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2SA: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O2SA \\sim O2SB: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
4. Rigid body (RIGU) restrains
 O2SA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2SB, O2SA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) O3SA(0.7) O5S(0.5) O2SA(0.65) O1S(0.5) O3SB(0.3)
 H5S(0.5) O2SB(0.35)
6.a Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00B), C00X(H00C,H00D), C13(H13A,H13B), C12(H12A,H12B), C2(H2A,H2B),
  C3(H3A,H3B), C1(H1A,H1B), C32(H32A,H32B), C11(H11A,H11B), C21(H21A,H21B)
6.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N7(H7), C24(H24), C31(H31), C17(H17), C7(H7A), C30(H30), C5(H5),
 C15(H15), C27(H27)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              97768
_olex2_submission_special_instructions 'No special instructions were received'