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_1575793
_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 Mn O10 Rh'
_chemical_formula_sum            'C25 H23 F12 Mn O10 Rh'
_chemical_formula_weight         869.28
_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                101.809(2)
_cell_angle_beta                 99.237(2)
_cell_angle_gamma                98.528(2)
_cell_formula_units_Z            2
_cell_length_a                   9.338(2)
_cell_length_b                   11.050(3)
_cell_length_c                   17.240(4)
_cell_measurement_reflns_used    9599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.94
_cell_volume                     1688.2(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v.2016.9-0 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.976
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16425
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.486
_diffrn_reflns_theta_min         2.937
_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    0.978
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was 
used for absorption correction. 
wR2(int) was 0.0851 before and 0.0661 
after correction. The Ratio of 
minimum to maximum transmission 
is 0.8431. The \l/2 correction 
factor is not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.492
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0715
_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^)+16.1271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4714
_reflns_number_total             6131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04912a2.cif
_cod_data_source_block           Rhacac3Mnhfac2
_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               1575793
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.859
_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.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C20(H20), C6(H6), C21(H21)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90749
_shelx_fab_checksum              84120
_olex2_submission_special_instructions 'No special instructions were received'