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_7706726
_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 F Gd N7 O7, 3.5(H2 O), C2 H5 O'
_chemical_formula_sum            'C35 H45 Cl2 F Gd N7 O11.5'
_chemical_formula_weight         994.93
_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                 113.504(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.146(2)
_cell_length_b                   23.647(5)
_cell_length_c                   14.793(3)
_cell_measurement_reflns_used    5101
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.28
_cell_volume                     3896.3(13)
_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
_diffrn_measured_fraction_theta_full 0.999
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27817
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.722
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0943 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.8184. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       plate
_exptl_crystal_F_000             2012
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dimethoxyethane diffusion into aqueous solution'
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.547
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.131
_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     561
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0468P)^2^+9.2272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6353
_reflns_number_total             8591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00616a2.cif
_cod_data_source_block           eb2003
_cod_depositor_comments
'Adding full bibliography for 7706725--7706728.cif.'
_cod_original_cell_volume        3896.5(14)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C35 H45 Cl2 F Gd N7 O11.50'
_cod_database_code               7706726
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.555
_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 C(H,H,H,H,H,H,H) groups, All O(H,H,H,H,H) groups
2. Restrained distances
 C2S-C2S_$1
 1.5 with sigma of 0.02
 H2SD-H2SC
 1.5 with sigma of 0.02
 H3SB-H3SA
 1.5 with sigma of 0.02
 O3S-H3SA = O3S-H3SB
 0.95 with sigma of 0.02
 O2S-H2SD = O2S-H2SC
 0.95 with sigma of 0.02
 O4SA-H4SA
 0.95 with sigma of 0.02
 O4SA-H4SC
 0.95 with sigma of 0.02
 H4SA-H4SC
 1.5 with sigma of 0.02
 O5S-H5S = O4SB-H5S
 0.95 with sigma of 0.02
 O5S-H5SA
 0.95 with sigma of 0.02
 H5S-H5SA
 1.5 with sigma of 0.02
 O4SB-H4SB
 0.95 with sigma of 0.02
 H4SB-H5S
 1.5 with sigma of 0.02
 O1S-C2S = O1S-C1S
 1.5 with sigma of 0.02
 H1SA-H5 \\sim H5-H1SB
 with sigma of 0.02
 O1S-C1S \\sim O1S-C2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1S \\sim C1S \\sim C2S: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 O1S, C1S, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O5S(0.5) O4SB(0.5) O4SA(0.5) H4SA(0.5) H4SC(0.5) H5SA(0.5) H4SB(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C20(H20A,H20B), C19(H19A,H19B), C10(H10A,H10B), C21(H21A,
 H21B), C2(H2A,H2B), C12(H12A,H12B), C3(H3A,H3B), C1(H1A,H1B), C32(H32A,H32B),
 C2S(H2SA,H2SB)
6.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N7(H7), C24(H24), C30(H30), C7(H7A), C27(H27), C31(H31), C5(H5),
 C16(H16), C14(H14)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              26597
_olex2_submission_special_instructions 'No special instructions were received'