Molecular precursor synthesis of the Rh<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>O<sub>3</sub> spherical architecture for enhanced acidic HER activity and durability.
Zulqarnain, Muhammad; Wei, Zheng; Hollo, Marcell; Dunn, Kathleen A.; Dikarev, Evgeny V.; Chemical science 16 (2025) 18695–18704; doi:10.1039/d5sc04912a

data_1575795
_publ_section_title
;
 Molecular precursor synthesis of the
 Rh<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>O<sub>3</sub> spherical
 architecture for enhanced acidic HER activity and durability.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              18695
_journal_page_last               18704
_journal_paper_doi               10.1039/d5sc04912a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C25 H23 F12 Fe O10 Rh'
_chemical_formula_sum            'C25 H23 F12 Fe O10 Rh'
_chemical_formula_weight         870.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-02-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-30 deposited with the CCDC.	2025-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.427(3)
_cell_angle_beta                 100.816(2)
_cell_angle_gamma                98.018(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3525(7)
_cell_length_b                   10.8615(8)
_cell_length_c                   17.1401(14)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.99
_cell_measurement_theta_min      2.97
_cell_volume                     1647.8(2)
_computing_cell_refinement       'SAINT V.8.37A (Bruker AXS Inc., 2016)'
_computing_data_collection       'APEX3 v.2016.9-0 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V.8.37A (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Xshell v.6.3.1 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v.2016.9-0 (Bruker AXS Inc., 2016)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.060
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.6958
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was 
used for absorption correction. 
wR2(int) was 0.0843 before 
and 0.0640 after correction. 
The Ratio of minimum to maximum 
transmission is 0.8625. 
The \l/2 correction factor is not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         14529
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+3.8674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11293
_reflns_number_total             14529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04912a2.cif
_cod_data_source_block           Rh(acac)3Fe(hfac)2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1575793--1575796.cif.
;
_cod_database_code               1575795
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.647
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C25 \\sim F9 \\sim F11 \\sim F12 \\sim F9X \\sim F11X \\sim F12X: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C25, F9, F11, F12, F9X, F11X, F12X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F9X)=Sof(F11X)=Sof(F12X)=1-FVAR(1)
 Sof(F9)=Sof(F11)=Sof(F12)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C19(H19), C20(H20)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9407
_shelx_fab_checksum              83395
_olex2_submission_special_instructions 'No special instructions were received'