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_7712600
_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         'C24 H32 Co2 N16 O8 S2, 2(B H3 O3)'
_chemical_formula_sum            'C24 H38 B2 Co2 N16 O14 S2'
_chemical_formula_weight         978.30
_chemical_name_systematic        22
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-10
_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                76.555(2)
_cell_angle_beta                 87.681(3)
_cell_angle_gamma                82.367(3)
_cell_formula_units_Z            1
_cell_length_a                   9.1985(7)
_cell_length_b                   9.6099(6)
_cell_length_c                   11.5412(7)
_cell_measurement_reflns_used    4368
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.20
_cell_volume                     983.40(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.993
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20328
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         2.508
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0115
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0622 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.4167.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear pinkish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 2652 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.582
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.4192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                6307
_reflns_number_total             7949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00196b2.cif
_cod_data_source_block           lwwwww
_cod_database_code               7712600
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.637
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 N6-H6
 0.88 with sigma of 0.02
 O13-H13A
 0.89 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N8(H8), N10(H10), N12(H12), N14(H14), N16(H16), C1(H1),
 C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6A), C7(H7), C8(H8A), C9(H9), C10(H10A),
 C11(H11), C12(H12A), C13(H13), C14(H14A), C15(H15), C16(H16A), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
3.b Idealised tetrahedral OH refined as rotating group:
 O9(H9A), O10(H10B), O11(H11A), O12(H12B), O14(H14B)
;
_shelx_res_checksum              99670
_shelx_hkl_checksum              25620
_olex2_submission_special_instructions 'No special instructions were received'