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_1575794
_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 Co F12 O10 Rh'
_chemical_formula_sum            'C25 H23 Co F12 O10 Rh'
_chemical_formula_weight         873.27
_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             2019-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-06-30 deposited with the CCDC.	2025-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.894(2)
_cell_angle_beta                 101.188(2)
_cell_angle_gamma                98.108(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3721(8)
_cell_length_b                   10.8813(9)
_cell_length_c                   17.0276(15)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.65
_cell_measurement_theta_min      2.95
_cell_volume                     1637.0(2)
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_collection       'APEX3 v.2016.9-0 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (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 0.998
_diffrn_measured_fraction_theta_max 0.984
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_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            39788
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.684
_diffrn_reflns_theta_min         2.946
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was 
used for absorption correction. 
wR2(int) was 0.0641 before and 0.0501 
after correction. The Ratio of 
minimum to maximum transmission 
is 0.8459. The \l/2 correction 
factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         14903
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0163P)^2^+2.6378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11725
_reflns_number_total             14903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04912a2.cif
_cod_data_source_block           Rh(acac)3Co(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               1575794
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.814
_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. Restrained distances
 F00H-C01D \\sim F0AA-C01D
 with sigma of 0.02
 F00M-C01D \\sim F1AA-C01D
 with sigma of 0.02
 F00N-C01D \\sim F2AA-C01D
 with sigma of 0.02
 F00M-C01D \\sim F1AA-C01D \\sim F00N-C01D \\sim F2AA-C01D \\sim F00H-C01D
\\sim F0AA-C01D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F00H \\sim F00M \\sim F00N \\sim C01D \\sim F0AA \\sim F1AA \\sim F2AA: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F00H, F00M, F00N, C01D, F0AA, F1AA, F2AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F0AA)=Sof(F1AA)=Sof(F2AA)=1-FVAR(1)
 Sof(F00H)=Sof(F00M)=Sof(F00N)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00V(H00V), C00Y(H00Y), C019(H019), C01A(H01M)
6.b Idealised Me refined as rotating group:
 C00Z(H00A,H00B,H00C), C010(H01A,H01B,H01C), C012(H01D,H01E,H01F), C014(H01G,
 H01H,H01I), C018(H01J,H01K,H01L), C01B(H01N,H01O,H01P)
;
_shelx_res_checksum              93959
_shelx_fab_checksum              23274
_olex2_submission_special_instructions 'No special instructions were received'