Iron(II)-α-keto acid complexes of tridentate ligands on gold nanoparticles: the effect of ligand geometry and immobilization on their dioxygen-dependent reactivity.
Bera, Abhijit; Sheet, Debobrata; Paine, Tapan Kanti; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1062–1073; doi:10.1039/d2dt02433k

data_7711887
_publ_section_title
;
 Iron(II)-&#x3b1;-keto acid complexes of tridentate ligands on gold
 nanoparticles: the effect of ligand geometry and immobilization on their
 dioxygen-dependent reactivity.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1062
_journal_page_last               1073
_journal_paper_doi               10.1039/d2dt02433k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C15 H19 Cl2 Fe N3'
_chemical_formula_sum            'C15 H19 Cl2 Fe N3'
_chemical_formula_weight         368.08
_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   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2ck9v3
_audit_creation_date             2022-07-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-19 deposited with the CCDC.	2022-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.845(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.655(5)
_cell_length_b                   12.892(7)
_cell_length_c                   14.631(8)
_cell_measurement_reflns_used    6208
_cell_measurement_temperature    99.96
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.36
_cell_volume                     1630.5(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.946
_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  0.0882
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12748
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.148
_diffrn_reflns_theta_min         2.356
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0997 after correction.
The Ratio of minimum to maximum transmission is 0.6914.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2768
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1054
_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^)+(0.1000P)^2^+27.9412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2614
_refine_ls_wR_factor_ref         0.2758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2235
_reflns_number_total             2768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02433k2.cif
_cod_data_source_block           mo_tkp070218_0m
_cod_depositor_comments
;
Adding full bibliography for 7711887--7711888.cif.

2025-03-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C3.33 H4.22 Cl0.44 Fe0.22 N0.67'
_cod_original_formula_weight         81.80
_cod_original_formula_moiety         '0.222(C15 H19 Cl2 Fe N3)'
_cod_original_formula_units_Z            18
_cod_original_cell_volume        1630.3(15)
_cod_database_code               7711887
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.974
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.967(2)
 0.033(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C8)
4. Rigid body (RIGU) restrains
 C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C10(H10), C3(H3), C4(H4), C11(H11)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              80870
_shelx_hkl_checksum              61893
_olex2_submission_special_instructions 'No special instructions were received'