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_7706725
_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         'C33 H35 F Gd N7 O7, 5(H2 O)'
_chemical_formula_sum            'C33 H45 F Gd N7 O12'
_chemical_formula_weight         908.01
_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   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                 107.6300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7854(3)
_cell_length_b                   24.3061(6)
_cell_length_c                   14.2062(3)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.25
_cell_volume                     3549.25(15)
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            219498
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.605
_diffrn_reflns_theta_min         1.722
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1366 before and 0.0542 after correction. The Ratio of minimum to maximum transmission is 0.8377. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       plate
_exptl_crystal_F_000             1844
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diffusion of glyme in aqueous solution'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10915
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+4.5759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9864
_reflns_number_total             10915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00616a2.cif
_cod_data_source_block           eb1917
_cod_depositor_comments
'Adding full bibliography for 7706725--7706728.cif.'
_cod_database_code               7706725
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.273
_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,H,H,H,H,H,H,H,H,H,H,H) groups
2. Restrained distances
 O3S-H3SA = O3S-H3SB
 0.95 with sigma of 0.02
 O5SB-H5SA
 0.95 with sigma of 0.02
 O5SB-H5SC
 0.95 with sigma of 0.02
 H5SD-O5SA
 0.95 with sigma of 0.02
 H5SA-H5SC
 1.5 with sigma of 0.02
 H3SA-O2S
 1.9 with sigma of 0.02
 H2SB-H2SA
 1.5 with sigma of 0.02
 O5SA-H5SC
 0.95 with sigma of 0.02
 O5SA-H5SD
 0.95 with sigma of 0.02
 O5SB-H5SD
 0.95 with sigma of 0.02
 H5SC-H5SD
 1.5 with sigma of 0.02
 H5SD-H5SA
 1.5 with sigma of 0.02
 O1S-H1SA
 0.95 with sigma of 0.02
 O1S-H1SB
 0.95 with sigma of 0.02
 O3S-H3SB
 0.95 with sigma of 0.02
 O3S-H3SA
 0.95 with sigma of 0.02
 O2S-H2SB
 0.95 with sigma of 0.02
 O2S-H2SA
 0.95 with sigma of 0.02
 O4S-H4SB
 0.95 with sigma of 0.02
 O4S-H4SA
 0.95 with sigma of 0.02
 O5SB-H5SB
 0.95 with sigma of 0.02
 H5SA-H5SB
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: O5SB(0.75) O5SA(0.25) H5SA(0.75) H5SC(0.25) H5SD(0.25) H5SB(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C3(H3A,H3B), C21(H21A,H21B), C20(H20A,H20B), C2(H2A,H2B),
 C11(H11A,H11B), C12(H12A,H12B), C1(H1A,H1B), C10(H10A,H10B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N6(H6), C25(H25), C31(H31), C24(H24), C15(H15), C28(H28), C16(H16),
 C5(H5), C7(H7A), C14(H14), C6(H6A)
4.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              79015
_olex2_submission_special_instructions 'No special instructions were received'