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_7706727
_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 H33 Cl2.5 Eu N7 O7.5, 1.5(H2 O), 0.5(Cl), H1.5 O, 1.5(O)'
_chemical_formula_sum            'C33 H37.5 Cl3 Eu N7 O11.5'
_chemical_formula_weight         974.51
_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
;
2021-02-23 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.684(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.126(4)
_cell_length_b                   23.598(7)
_cell_length_c                   14.735(4)
_cell_measurement_reflns_used    6011
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22.69
_cell_measurement_theta_min      2.29
_cell_volume                     3861(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.1213
_diffrn_reflns_av_unetI/netI     0.0919
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43327
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.061
_diffrn_reflns_theta_min         1.738
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1436 before and 0.0714 after correction. The Ratio of minimum to maximum transmission is 0.8433. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.910
_refine_diff_density_min         -2.253
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         7600
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0354P)^2^+34.9160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5340
_reflns_number_total             7600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00616a2.cif
_cod_data_source_block           eb2007
_cod_depositor_comments
'Adding full bibliography for 7706725--7706728.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C33 H37.50 Cl3 Eu N7 O11.50'
_cod_database_code               7706727
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.395
_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) groups, All O(H,H,H,H) groups
2. Shared sites
{Cl0A, O1S}
3. Restrained distances
 O5SA-H5SB
 0.95 with sigma of 0.02
 O5SA-H5SA
 0.95 with sigma of 0.02
 H5SB-H5SA
 1.5 with sigma of 0.02
 O3SB-H3SA
 0.95 with sigma of 0.02
 O2SA-H2SA = O2SA-H2SB
 0.95 with sigma of 0.02
 H2SB-H2SA
 1.5 with sigma of 0.02
 O3SB-H3SB
 0.95 with sigma of 0.02
 H3SA-H3SB
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C18)
Uanis(Cl1) = Uanis(Cl2)
Uanis(Cl0A) = Uanis(O1S)
5. Others
 Fixed Sof: Cl1A(0.5) O3SB(0.5) O3SA(0.5) O4SA(0.5) O2SA(0.5) O2SB(0.5)
 O5SB(0.5) H3SA(0.5) H2SA(0.5) H2SB(0.5) Cl0A(0.5) O1S(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C1(H1A,H1B), C2(H2A,H2B), C12(H12A,H12B), C3(H3A,H3B),
 C20(H20A,H20B), C10(H10A,H10B), C19(H19A,H19B), C32(H32A,H32B), C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N7(H7), C31(H31), C16(H16), C24(H24), C25(H25), C28(H28), C7(H7A),
 C5(H5), C14(H14)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              59653
_olex2_submission_special_instructions 'No special instructions were received'