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#$Date: 2024-07-05 18:23:30 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248397.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_7248397
loop_
_publ_author_name
'Sofronova, Svetlana'
'Moshkina, Evgeniya'
'Chernyshev, Artem'
'Vasiliev, Aleksandr'
'Maximov, Nikolai G.'
'Aleksandrovsky, Aleksandr'
'Andryushchenko, Tatyana'
'Shabanov, Aleksandr'
_publ_section_title
;
 Crystal growth and cation order of Ni3−xCoxB2O6 oxyborates
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2536
_journal_page_last               2543
_journal_paper_doi               10.1039/D4CE00091A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'B4 Co1.76 Ni4.24 O12'
_chemical_formula_sum            'B4 Co1.76 Ni4.24 O12'
_chemical_formula_weight         587.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-30 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   4.4917(6)
_cell_length_b                   5.4314(8)
_cell_length_c                   8.3789(12)
_cell_measurement_reflns_used    2438
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      38.72
_cell_measurement_theta_min      3.75
_cell_volume                     204.41(5)
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker PHOTON-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3844
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.996
_diffrn_reflns_theta_min         4.472
_exptl_absorpt_coefficient_mu    13.136
_exptl_absorpt_correction_T_max  0.141
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.775
_exptl_crystal_description       shapeless
_exptl_crystal_F_000             282.2
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.271(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0288
_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/[σ²(Fo²)+(0.0387P)²+0.1986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                525
_reflns_number_total             584
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00091a1.cif
_cod_data_source_block           6_0m_a
_cod_depositor_comments          'Adding full bibliography for 7248397.cif.'
_cod_database_code               7248397
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
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
Ni1 Ni 0.000000 0.500000 0.81521(4) 0.00514(14) Uani 0.66(13) 2 d S T P . .
Co1 Co 0.000000 0.500000 0.81521(4) 0.00514(14) Uani 0.34(13) 2 d S T P . .
Ni2 Ni 0.500000 0.500000 0.500000 0.00516(16) Uani 0.80(15) 4 d S T P . .
Co2 Co 0.500000 0.500000 0.500000 0.00516(16) Uani 0.20(15) 4 d S T P . .
O1 O 0.2014(2) 0.29748(19) 0.63965(14) 0.0065(3) Uani 1 1 d . . . . .
O2 O 0.7476(3) 0.1771(3) 0.500000 0.0061(3) Uani 1 2 d S T P . .
B B 1.0428(5) 0.2458(4) 0.500000 0.0062(4) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 O1 88.15(7) . 2_565 ?
O1 Ni1 O2 92.80(5) . 7_566 ?
O1 Ni1 O2 173.26(5) 2_565 7_566 ?
O1 Ni1 O2 173.26(5) . 3_556 ?
O1 Ni1 O2 92.80(5) 2_565 3_556 ?
O2 Ni1 O2 87.04(6) 7_566 3_556 ?
O1 Ni1 O1 104.86(3) . 3_556 ?
O1 Ni1 O1 89.90(3) 2_565 3_556 ?
O2 Ni1 O1 83.41(5) 7_566 3_556 ?
O2 Ni1 O1 81.82(5) 3_556 3_556 ?
O1 Ni1 O1 89.90(3) . 4_456 ?
O1 Ni1 O1 104.86(3) 2_565 4_456 ?
O2 Ni1 O1 81.82(5) 7_566 4_456 ?
O2 Ni1 O1 83.41(5) 3_556 4_456 ?
O1 Ni1 O1 159.58(6) 3_556 4_456 ?
O2 Ni2 O2 180.0 . 5_666 ?
O2 Ni2 O1 84.22(4) . 6_556 ?
O2 Ni2 O1 95.78(4) 5_666 6_556 ?
O2 Ni2 O1 95.78(4) . 2_665 ?
O2 Ni2 O1 84.22(4) 5_666 2_665 ?
O1 Ni2 O1 180.0 6_556 2_665 ?
O2 Ni2 O1 95.78(4) . 5_666 ?
O2 Ni2 O1 84.22(4) 5_666 5_666 ?
O1 Ni2 O1 112.00(6) 6_556 5_666 ?
O1 Ni2 O1 68.00(6) 2_665 5_666 ?
O2 Ni2 O1 84.22(4) . . ?
O2 Ni2 O1 95.78(4) 5_666 . ?
O1 Ni2 O1 68.01(6) 6_556 . ?
O1 Ni2 O1 111.99(6) 2_665 . ?
O1 Ni2 O1 180.0 5_666 . ?
O2 Ni2 B 91.54(7) . 5_766 ?
O2 Ni2 B 88.46(7) 5_666 5_766 ?
O1 Ni2 B 145.62(3) 6_556 5_766 ?
O1 Ni2 B 34.38(3) 2_665 5_766 ?
O1 Ni2 B 34.38(3) 5_666 5_766 ?
O1 Ni2 B 145.62(3) . 5_766 ?
O2 Ni2 B 88.46(7) . 1_455 ?
O2 Ni2 B 91.54(7) 5_666 1_455 ?
O1 Ni2 B 34.38(3) 6_556 1_455 ?
O1 Ni2 B 145.62(3) 2_665 1_455 ?
O1 Ni2 B 145.62(3) 5_666 1_455 ?
O1 Ni2 B 34.38(3) . 1_455 ?
B Ni2 B 180.0 5_766 1_455 ?
B O1 Ni1 118.95(11) 1_455 . ?
B O1 Ni2 87.95(10) 1_455 . ?
Ni1 O1 Ni2 113.74(5) . . ?
B O1 Ni1 108.45(11) 1_455 3_546 ?
Ni1 O1 Ni1 123.86(6) . 3_546 ?
Ni2 O1 Ni1 95.41(4) . 3_546 ?
B O2 Ni2 106.67(13) . . ?
B O2 Ni1 128.56(6) . 7_665 ?
Ni2 O2 Ni1 95.83(5) . 7_665 ?
B O2 Ni1 128.56(6) . 3_546 ?
Ni2 O2 Ni1 95.83(5) . 3_546 ?
Ni1 O2 Ni1 92.96(6) 7_665 3_546 ?
O2 B O1 123.01(9) . 1_655 ?
O2 B O1 123.01(9) . 6_656 ?
O1 B O1 113.60(18) 1_655 6_656 ?
O2 B Ni2 161.79(16) . 1_655 ?
O1 B Ni2 57.67(9) 1_655 1_655 ?
O1 B Ni2 57.67(9) 6_656 1_655 ?
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
Ni1 O1 2.0475(11) . ?
Ni1 O1 2.0475(11) 2_565 ?
Ni1 O2 2.1352(10) 7_566 ?
Ni1 O2 2.1352(10) 3_556 ?
Ni1 O1 2.1337(11) 3_556 ?
Ni1 O1 2.1337(11) 4_456 ?
Ni2 O2 2.0767(15) . ?
Ni2 O2 2.0767(15) 5_666 ?
Ni2 O1 2.0923(11) 6_556 ?
Ni2 O1 2.0923(11) 2_665 ?
Ni2 O1 2.0923(11) 5_666 ?
Ni2 O1 2.0924(11) . ?
Ni2 B 2.475(2) 5_766 ?
Ni2 B 2.475(2) 1_455 ?
O1 B 1.3984(17) 1_455 ?
O2 B 1.378(3) . ?
