Exploration of the oxygen reduction reaction activity of four transition metal borates: synthesis, structure and characterization.
Deng, Yan-Ling; Chen, An-Na; Li, Wei; Xin, Shu-Sheng; Pan, Chun-Yang; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00196b

data_7712599
_publ_section_title
;
 Exploration of the oxygen reduction reaction activity of four transition
 metal borates: synthesis, structure and characterization.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00196b
_journal_year                    2023
_chemical_formula_moiety         'B6.5 Co0.5 H3 O13.5, 1.4(K2.5), 0.5(O)'
_chemical_formula_sum            'B6.5 Co0.5 H3 K3.5 O14'
_chemical_formula_weight         463.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-10 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3437(6)
_cell_length_b                   9.1086(4)
_cell_length_c                   12.9438(6)
_cell_measurement_reflns_used    3368
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.73
_cell_volume                     1455.32(12)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15471
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.391
_diffrn_reflns_theta_min         1.573
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0112
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0667 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.4058.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.972
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
;
 Flack x determined using 1091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3105
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0946P)^2^+3.9513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                2695
_reflns_number_total             3105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00196b2.cif
_cod_data_source_block           11
_cod_original_formula_sum        'B6.50 H3 Co0.50 K3.50 O14'
_cod_database_code               7712599
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.596
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(6)
 0.46(6)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
3. Rigid bond restraints
 O1W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H9(0.5) H13(0.5)
6.a Tetrahedral OH refined with riding coordinates:
 O10(H10), O14(H14), O13(H13)
6.b Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              78883
_shelx_hkl_checksum              93508
_olex2_submission_original_sample_id 11
_olex2_submission_special_instructions 'No special instructions were received'