#------------------------------------------------------------------------------
#$Date: 2023-03-14 01:59:07 +0200 (Tue, 14 Mar 2023) $
#$Revision: 281852 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/25/7712598.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712598
loop_
_publ_author_name
'Deng, Yan-Ling'
'Chen, An-Na'
'Li, Wei'
'Xin, Shu-Sheng'
'Pan, Chun-Yang'
_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         '0.13(C16 H30 B10 Co2 N8 O20)'
_chemical_formula_sum            'C2 H3.75 B1.25 Co0.25 N O2.5'
_chemical_formula_weight         110.05
_chemical_name_systematic        S1
_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
_audit_creation_date             2022-03-01
_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                91.927(4)
_cell_angle_beta                 102.862(3)
_cell_angle_gamma                115.726(3)
_cell_formula_units_Z            8
_cell_length_a                   8.9576(10)
_cell_length_b                   9.4001(11)
_cell_length_c                   11.9155(12)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.43
_cell_volume                     871.44(17)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16946
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.432
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0108
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0560 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.3913.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       plate
_exptl_crystal_F_000             446
_exptl_crystal_preparation       1
_exptl_crystal_recrystallization_method 1
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0282
_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/[σ²(Fo²)+(0.0309P)²+0.5646P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3296
_reflns_number_total             3563
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00196b2.cif
_cod_data_source_block           ss12
_cod_original_formula_sum        'C2 H3.75 B1.25 Co0.25 N O2.50'
_cod_database_code               7712598
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.623
_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, All O(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C5(H5), C6(H6), C7(H7)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
3.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O10(H10)
;
_olex2_exptl_crystal_mounting_method 1
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.88233(3) 0.54900(3) 0.53917(2) 0.02582(9) Uani 1 1 d . U . . .
O1 O 0.8719(2) 0.40284(19) 0.41390(13) 0.0386(3) Uani 1 1 d . U . . .
O2 O 0.7744(2) 0.19888(19) 0.25862(13) 0.0390(4) Uani 1 1 d . U . . .
O3 O 0.6906(2) -0.00215(19) 0.10473(13) 0.0379(3) Uani 1 1 d . U . . .
H3 H 0.618328 -0.044923 0.040081 0.057 Uiso 1 1 calc GR . . . .
O4 O 0.6138(2) 0.34308(19) 0.27094(14) 0.0412(4) Uani 1 1 d . U . . .
O5 O 0.52221(19) 0.13590(18) 0.10755(13) 0.0370(3) Uani 1 1 d . U . . .
O6 O 0.3202(2) 0.1477(2) 0.20472(14) 0.0408(4) Uani 1 1 d . U . . .
O7 O 0.4448(2) 0.34801(19) 0.08487(14) 0.0389(3) Uani 1 1 d . U . . .
O8 O 0.0269(2) 0.0309(2) 0.18755(15) 0.0453(4) Uani 1 1 d . U . . .
H8 H -0.063159 0.031654 0.148565 0.068 Uiso 1 1 calc GR . . . .
O9 O 0.1416(2) 0.2170(2) 0.06063(15) 0.0452(4) Uani 1 1 d . U . . .
O10 O 0.2565(2) 0.4145(2) -0.05315(16) 0.0498(4) Uani 1 1 d . U . . .
H10 H 0.351151 0.480707 -0.062287 0.075 Uiso 1 1 calc GR . . . .
N1 N 0.8111(2) 0.7097(2) 0.48397(16) 0.0392(4) Uani 1 1 d . U . . .
N2 N 0.7877(3) 0.4553(2) 0.66907(17) 0.0410(4) Uani 1 1 d . U . . .
N3 N 0.7638(3) 0.9188(2) 0.4955(2) 0.0469(5) Uani 1 1 d . U . . .
N4 N 0.7713(3) 0.3440(2) 0.82784(17) 0.0415(4) Uani 1 1 d . U . . .
C1 C 0.8277(3) 0.7779(3) 0.3834(2) 0.0469(6) Uani 1 1 d . U . . .
H1 H 0.854249 0.739492 0.319484 0.056 Uiso 1 1 calc R . . . .
C2 C 0.8003(3) 0.9077(3) 0.3907(2) 0.0522(6) Uani 1 1 d . U . . .
H2 H 0.805201 0.977567 0.334318 0.063 Uiso 1 1 calc R . . . .
C3 C 0.7720(3) 0.7991(3) 0.5488(2) 0.0419(5) Uani 1 1 d . U . . .
H3A H 0.752446 0.780276 0.623295 0.050 Uiso 1 1 calc R . . . .
C4 C 0.7294(4) 1.0428(3) 0.5440(3) 0.0681(9) Uani 1 1 d . U . . .
H4A H 0.695418 1.015294 0.616037 0.102 Uiso 1 1 calc GR . . . .
H4B H 0.636450 1.051046 0.487653 0.102 Uiso 1 1 calc GR . . . .
H4C H 0.833338 1.145308 0.560687 0.102 Uiso 1 1 calc GR . . . .
C5 C 0.6297(3) 0.4176(3) 0.6884(2) 0.0473(6) Uani 1 1 d . U . . .
H5 H 0.542278 0.437007 0.640575 0.057 Uiso 1 1 calc R . . . .
C6 C 0.6183(3) 0.3487(3) 0.7859(2) 0.0475(6) Uani 1 1 d . U . . .
H6 H 0.523195 0.310989 0.818866 0.057 Uiso 1 1 calc R . . . .
C7 C 0.8688(3) 0.4086(3) 0.7565(2) 0.0410(5) Uani 1 1 d . U . . .
H7 H 0.981880 0.420186 0.766416 0.049 Uiso 1 1 calc R . . . .
C8 C 0.8182(4) 0.2772(3) 0.9315(2) 0.0524(6) Uani 1 1 d . U . . .
H8A H 0.936938 0.294059 0.943689 0.079 Uiso 1 1 calc GR . . . .
H8B H 0.741107 0.162499 0.920573 0.079 Uiso 1 1 calc GR . . . .
H8C H 0.808003 0.330322 0.999511 0.079 Uiso 1 1 calc GR . . . .
B1 B 0.7500(3) 0.3170(3) 0.3149(2) 0.0339(5) Uani 1 1 d . U . . .
B2 B 0.6587(3) 0.1106(3) 0.1551(2) 0.0330(5) Uani 1 1 d . U . . .
B3 B 0.4746(3) 0.2455(3) 0.1690(2) 0.0371(5) Uani 1 1 d . U . . .
B4 B 0.1629(3) 0.1308(3) 0.1496(2) 0.0385(5) Uani 1 1 d . U . . .
B5 B 0.2842(3) 0.3276(3) 0.0310(2) 0.0401(6) Uani 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 41.19(4) 2_766 2_766 ?
O1 Co1 Co1 41.98(5) . 2_766 ?
O1 Co1 O1 83.17(7) . 2_766 ?
O1 Co1 N1 113.64(7) . . ?
O1 Co1 N2 117.50(8) . . ?
N1 Co1 Co1 128.08(6) . 2_766 ?
N1 Co1 O1 121.38(8) . 2_766 ?
N1 Co1 N2 112.73(8) . . ?
N2 Co1 Co1 119.11(6) . 2_766 ?
N2 Co1 O1 105.52(7) . 2_766 ?
Co1 O1 Co1 96.83(7) . 2_766 ?
B1 O1 Co1 133.06(15) . . ?
B1 O1 Co1 129.18(15) . 2_766 ?
B2 O2 B1 119.29(18) . . ?
B1 O4 B3 124.02(18) . . ?
B2 O5 B3 122.94(17) . . ?
B4 O6 B3 122.91(19) . . ?
B5 O7 B3 122.4(2) . . ?
B5 O9 B4 119.50(19) . . ?
C1 N1 Co1 127.94(16) . . ?
C3 N1 Co1 124.87(16) . . ?
C3 N1 C1 105.7(2) . . ?
C5 N2 Co1 130.00(16) . . ?
C7 N2 Co1 124.65(16) . . ?
C7 N2 C5 105.3(2) . . ?
C2 N3 C4 126.8(2) . . ?
C3 N3 C2 107.9(2) . . ?
C3 N3 C4 125.3(3) . . ?
C6 N4 C8 126.4(2) . . ?
C7 N4 C6 107.6(2) . . ?
C7 N4 C8 126.0(2) . . ?
C2 C1 N1 109.0(2) . . ?
C1 C2 N3 106.5(2) . . ?
N1 C3 N3 110.9(2) . . ?
C6 C5 N2 109.3(2) . . ?
C5 C6 N4 106.4(2) . . ?
N4 C7 N2 111.3(2) . . ?
O1 B1 O2 116.0(2) . . ?
O4 B1 O1 122.9(2) . . ?
O4 B1 O2 121.0(2) . . ?
O3 B2 O2 116.18(19) . . ?
O5 B2 O2 121.1(2) . . ?
O5 B2 O3 122.7(2) . . ?
O4 B3 O5 110.42(18) . . ?
O4 B3 O7 110.11(19) . . ?
O6 B3 O4 109.82(19) . . ?
O6 B3 O5 108.03(19) . . ?
O6 B3 O7 111.82(18) . . ?
O7 B3 O5 106.57(18) . . ?
O6 B4 O8 117.7(2) . . ?
O6 B4 O9 121.2(2) . . ?
O8 B4 O9 121.0(2) . . ?
O7 B5 O9 120.8(2) . . ?
O10 B5 O7 122.1(2) . . ?
O10 B5 O9 117.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.9441(6) 2_766 ?
Co1 O1 1.9528(15) . ?
Co1 O1 1.9832(16) 2_766 ?
Co1 N1 1.9588(19) . ?
Co1 N2 1.979(2) . ?
O1 B1 1.354(3) . ?
O2 B1 1.398(3) . ?
O2 B2 1.378(3) . ?
O3 B2 1.364(3) . ?
O4 B1 1.345(3) . ?
O4 B3 1.459(3) . ?
O5 B2 1.351(3) . ?
O5 B3 1.499(3) . ?
O6 B3 1.458(3) . ?
O6 B4 1.352(3) . ?
O7 B3 1.474(3) . ?
O7 B5 1.364(3) . ?
O8 B4 1.361(3) . ?
O9 B4 1.385(3) . ?
O9 B5 1.382(3) . ?
O10 B5 1.362(3) . ?
N1 C1 1.385(3) . ?
N1 C3 1.326(3) . ?
N2 C5 1.378(3) . ?
N2 C7 1.332(3) . ?
N3 C2 1.371(4) . ?
N3 C3 1.332(3) . ?
N3 C4 1.461(3) . ?
N4 C6 1.370(3) . ?
N4 C7 1.327(3) . ?
N4 C8 1.465(3) . ?
C1 C2 1.349(4) . ?
C5 C6 1.352(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O5 0.84 1.84 2.678(2) 174.3 2_655 yes
O8 H8 O3 0.84 2.03 2.826(2) 159.0 1_455 yes
O10 H10 O7 0.84 1.92 2.758(2) 172.4 2_665 yes
