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_7712601
_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_absolute_configuration ad
_chemical_formula_moiety         '0.04(C112 H98 B4 K4 N16 Ni8 O48)'
_chemical_formula_sum            'C4.48 H3.92 B0.16 K0.16 N0.64 Ni0.32 O1.92'
_chemical_formula_weight         124.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 115.1050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            25
_cell_length_a                   9.6192(2)
_cell_length_b                   33.4680(7)
_cell_length_c                   10.6609(3)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.20
_cell_volume                     3107.89(13)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0673
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            62596
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         2.416
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0109
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0775 after correction.
The Ratio of minimum to maximum transmission is 0.3949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 4976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12666
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.2841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                11674
_reflns_number_total             12666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00196b2.cif
_cod_data_source_block           d4
_cod_database_code               7712601
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C34(H34), C2(H2), C7(H7), C6(H6), C31(H31), C3(H3), C30(H30), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C50(H50), C15(H15), C19(H19), C44(H44), C46(H46),
 C52(H52), C21(H21), C13(H13), C10(H10), C37(H37), C51(H51), C42(H42), C9(H9),
 C11(H11), C45(H45), C38(H38), C48(H48), C53(H53), C54(H54), C39(H39), C28(H28),
  C22(H22), C55(H55), C43(H43), C26(H26), C24(H24), C27(H27), C56(H56),
 C49(H49), C23(H23), C41(H41), C18(H18), C17(H17), C20(H20), C47(H47), C12(H12),
  C40(H40)
;
_shelx_res_checksum              92288
_shelx_hkl_checksum              26454
_olex2_submission_special_instructions 'No special instructions were received'