#------------------------------------------------------------------------------
#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/35/4323562.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_4323562
loop_
_publ_author_name
'Pingrong Wei'
'David A. Atwood'
_publ_section_title
;
 Bimetallic Borate Derivatives of the Salen Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4060
_journal_page_last               4065
_journal_paper_doi               10.1021/ic970089i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C25 H36 B2 N2 O6'
_chemical_formula_weight         482.18
_chemical_name_common            Salpen{B(OMe)2}2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                109.315(2)
_cell_angle_beta                 98.544(2)
_cell_angle_gamma                104.561(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6718(9)
_cell_length_b                   13.2311(13)
_cell_length_c                   13.3266(14)
_cell_measurement_temperature    298(2)
_cell_volume                     1351.0(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'SIEMENS CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5056
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.083
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       prism
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.145
_refine_ls_goodness_of_fit_obs   1.211
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_restrained_S_obs      1.211
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_obs          0.0719
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0251P)²+1.3299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1556
_refine_ls_wR_factor_obs         0.1346
_reflns_number_observed          2330
_reflns_number_total             3289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970089i_5.cif
_cod_data_source_block           j
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+1.3299P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+1.3299P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323562
loop_
_symmetry_equiv_pos_as_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
B1 B 0.1919(7) 0.7910(4) 0.2761(5) 0.0678(15) Uani 1 d . .
B2 B 0.2626(6) 1.2252(4) 0.1620(4) 0.0579(13) Uani 1 d . .
O1 O 0.1263(4) 0.8242(3) 0.3677(3) 0.0826(9) Uani 1 d . .
O2 O 0.3444(4) 0.8723(3) 0.2862(3) 0.0780(9) Uani 1 d . .
O3 O 0.2886(4) 1.1851(3) 0.0560(2) 0.0716(9) Uani 1 d . .
O4 O 0.0967(3) 1.2245(2) 0.1485(2) 0.0646(8) Uani 1 d . .
O5 O 0.2032(4) 0.6758(3) 0.2514(3) 0.0765(9) Uani 1 d . .
O6 O 0.3821(4) 1.3374(2) 0.2337(3) 0.0739(9) Uani 1 d . .
N1 N 0.0736(4) 0.7837(3) 0.1663(3) 0.0572(9) Uani 1 d . .
N2 N 0.2870(4) 1.1381(3) 0.2200(3) 0.0606(9) Uani 1 d . .
C1 C -0.0137(7) 0.7488(5) 0.3779(5) 0.094(2) Uani 1 d . .
H1A H 0.0123(7) 0.6832(5) 0.3828(5) 0.112 Uiso 1 calc R .
H1B H -0.1037(7) 0.7232(5) 0.3132(5) 0.112 Uiso 1 calc R .
C2 C -0.0650(9) 0.8056(5) 0.4774(5) 0.132(2) Uani 1 d . .
H2A H -0.1596(9) 0.7536(5) 0.4831(5) 0.198 Uiso 1 calc R .
H2B H -0.0921(9) 0.8700(5) 0.4720(5) 0.198 Uiso 1 calc R .
H2C H 0.0237(9) 0.8301(5) 0.5414(5) 0.198 Uiso 1 calc R .
C3 C 0.4890(8) 0.8776(6) 0.3547(6) 0.147(3) Uani 1 d . .
H3A H 0.5042(8) 0.8040(6) 0.3290(6) 0.177 Uiso 1 calc R .
H3B H 0.4747(8) 0.8940(6) 0.4286(6) 0.177 Uiso 1 calc R .
C4 C 0.6361(8) 0.9616(6) 0.3588(6) 0.151(3) Uani 1 d . .
H4A H 0.7291(8) 0.9603(6) 0.4068(6) 0.227 Uiso 1 calc R .
H4B H 0.6237(8) 1.0352(6) 0.3861(6) 0.227 Uiso 1 calc R .
H4C H 0.6533(8) 0.9451(6) 0.2864(6) 0.227 Uiso 1 calc R .
C5 C 0.4497(7) 1.1867(6) 0.0484(5) 0.114(2) Uani 1 d . .
H5A H 0.5217(7) 1.2646(6) 0.0802(5) 0.137 Uiso 1 calc R .
H5B H 0.4881(7) 1.1476(6) 0.0918(5) 0.137 Uiso 1 calc R .
C6 C 0.4627(9) 1.1375(8) -0.0574(6) 0.185(4) Uani 1 d . .
H6A H 0.5751(9) 1.1417(8) -0.0561(6) 0.277 Uiso 1 calc R .
H6B H 0.4278(9) 1.1769(8) -0.1007(6) 0.277 Uiso 1 calc R .
H6C H 0.3941(9) 1.0597(8) -0.0890(6) 0.277 Uiso 1 calc R .
C7 C 0.0462(6) 1.2758(4) 0.2432(4) 0.0862(15) Uani 1 d . .
H7A H 0.0835(6) 1.3571(4) 0.2643(4) 0.103 Uiso 1 calc R .
H7B H 0.0969(6) 1.2593(4) 0.3033(4) 0.103 Uiso 1 calc R .
C8 C -0.1339(7) 1.2349(6) 0.2239(6) 0.127(2) Uani 1 d . .
H8A H -0.1642(7) 1.2713(6) 0.2897(6) 0.191 Uiso 1 calc R .
H8B H -0.1708(7) 1.1546(6) 0.2043(6) 0.191 Uiso 1 calc R .
H8C H -0.1842(7) 1.2523(6) 0.1653(6) 0.191 Uiso 1 calc R .
C9 C 0.2214(5) 0.6172(4) 0.1534(5) 0.0679(13) Uani 1 d . .
C10 C 0.2911(6) 0.5316(4) 0.1429(5) 0.087(2) Uani 1 d . .
H10A H 0.3252(6) 0.5156(4) 0.2038(5) 0.104 Uiso 1 calc R .
C11 C 0.3091(7) 0.4721(5) 0.0445(7) 0.100(2) Uani 1 d . .
H11A H 0.3579(7) 0.4160(5) 0.0389(7) 0.119 Uiso 1 calc R .
C12 C 0.2576(7) 0.4914(4) -0.0484(6) 0.095(2) Uani 1 d . .
H12A H 0.2734(7) 0.4500(4) -0.1153(6) 0.114 Uiso 1 calc R .
C13 C 0.1821(6) 0.5731(4) -0.0410(4) 0.0784(14) Uani 1 d . .
H13A H 0.1438(6) 0.5853(4) -0.1035(4) 0.094 Uiso 1 calc R .
C14 C 0.1636(5) 0.6367(3) 0.0596(4) 0.0592(11) Uani 1 d . .
C15 C 0.0759(5) 0.7173(3) 0.0719(4) 0.0585(11) Uani 1 d . .
H15A H 0.0190(5) 0.7213(3) 0.0091(4) 0.070 Uiso 1 calc R .
C16 C -0.0314(5) 0.8564(3) 0.1726(4) 0.0697(13) Uani 1 d . .
H16A H -0.1111(5) 0.8381(3) 0.2131(4) 0.084 Uiso 1 calc R .
H16B H -0.0916(5) 0.8410(3) 0.0989(4) 0.084 Uiso 1 calc R .
C17 C 0.0672(6) 0.9810(3) 0.2281(4) 0.0712(13) Uani 1 d . .
H17A H -0.0078(6) 1.0249(3) 0.2369(4) 0.085 Uiso 1 calc R .
H17B H 0.1310(6) 0.9959(3) 0.3007(4) 0.085 Uiso 1 calc R .
C18 C 0.1818(6) 1.0183(3) 0.1632(4) 0.0707(13) Uani 1 d . .
H18A H 0.2516(6) 0.9708(3) 0.1500(4) 0.085 Uiso 1 calc R .
H18B H 0.1173(6) 1.0078(3) 0.0924(4) 0.085 Uiso 1 calc R .
C19 C 0.3982(6) 1.1681(4) 0.3093(4) 0.0690(13) Uani 1 d . .
H19A H 0.4065(6) 1.1138(4) 0.3378(4) 0.083 Uiso 1 calc R .
C20 C 0.5082(5) 1.2795(4) 0.3660(4) 0.0630(12) Uani 1 d . .
C21 C 0.4974(5) 1.3612(4) 0.3235(4) 0.0626(12) Uani 1 d . .
C22 C 0.6099(6) 1.4693(4) 0.3755(4) 0.0832(15) Uani 1 d . .
H22A H 0.6051(6) 1.5239(4) 0.3467(4) 0.100 Uiso 1 calc R .
C23 C 0.7287(7) 1.4962(5) 0.4695(5) 0.100(2) Uani 1 d . .
H23A H 0.8037(7) 1.5690(5) 0.5038(5) 0.120 Uiso 1 calc R .
C24 C 0.7376(8) 1.4161(5) 0.5134(5) 0.105(2) Uani 1 d . .
H24A H 0.8167(8) 1.4351(5) 0.5778(5) 0.126 Uiso 1 calc R .
C25 C 0.6297(7) 1.3094(5) 0.4617(4) 0.088(2) Uani 1 d . .
H25A H 0.6369(7) 1.2552(5) 0.4906(4) 0.105 Uiso 1 calc R .
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'
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 B1 O2 113.0(4) . . ?
O1 B1 O5 110.7(4) . . ?
O2 B1 O5 112.9(4) . . ?
O1 B1 N1 111.4(4) . . ?
O2 B1 N1 102.8(4) . . ?
O5 B1 N1 105.5(4) . . ?
O3 B2 O4 107.1(4) . . ?
O3 B2 O6 112.7(4) . . ?
O4 B2 O6 112.8(4) . . ?
O3 B2 N2 108.4(4) . . ?
O4 B2 N2 108.8(3) . . ?
O6 B2 N2 106.8(3) . . ?
B1 O1 C1 120.8(4) . . ?
C3 O2 B1 118.4(4) . . ?
B2 O3 C5 117.6(4) . . ?
C7 O4 B2 118.1(4) . . ?
C9 O5 B1 120.0(4) . . ?
C21 O6 B2 126.9(3) . . ?
C15 N1 C16 119.2(4) . . ?
C15 N1 B1 119.7(4) . . ?
C16 N1 B1 121.1(4) . . ?
C19 N2 C18 119.6(4) . . ?
C19 N2 B2 122.7(4) . . ?
C18 N2 B2 117.6(4) . . ?
O1 C1 C2 110.5(5) . . ?
O2 C3 C4 114.3(6) . . ?
C6 C5 O3 114.2(6) . . ?
O4 C7 C8 111.5(5) . . ?
O5 C9 C10 119.5(5) . . ?
O5 C9 C14 121.1(4) . . ?
C10 C9 C14 119.3(5) . . ?
C11 C10 C9 119.8(6) . . ?
C10 C11 C12 122.1(6) . . ?
C11 C12 C13 119.2(6) . . ?
C12 C13 C14 120.0(5) . . ?
C13 C14 C9 119.5(4) . . ?
C13 C14 C15 122.8(4) . . ?
C9 C14 C15 117.5(4) . . ?
N1 C15 C14 122.2(4) . . ?
N1 C16 C17 112.3(3) . . ?
C18 C17 C16 112.1(4) . . ?
N2 C18 C17 112.6(4) . . ?
N2 C19 C20 123.2(4) . . ?
C21 C20 C25 119.1(4) . . ?
C21 C20 C19 118.8(4) . . ?
C25 C20 C19 122.1(4) . . ?
O6 C21 C22 119.4(4) . . ?
O6 C21 C20 121.3(4) . . ?
C22 C21 C20 119.3(4) . . ?
C23 C22 C21 120.3(5) . . ?
C22 C23 C24 120.6(5) . . ?
C25 C24 C23 119.4(5) . . ?
C24 C25 C20 121.3(5) . . ?
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
B1 O1 1.409(6) . ?
B1 O2 1.435(6) . ?
B1 O5 1.480(6) . ?
B1 N1 1.616(6) . ?
B2 O3 1.410(6) . ?
B2 O4 1.421(5) . ?
B2 O6 1.478(6) . ?
B2 N2 1.623(5) . ?
O1 C1 1.421(6) . ?
O2 C3 1.408(6) . ?
O3 C5 1.411(6) . ?
O4 C7 1.410(5) . ?
O5 C9 1.337(5) . ?
O6 C21 1.329(5) . ?
N1 C15 1.281(5) . ?
N1 C16 1.474(5) . ?
N2 C19 1.286(5) . ?
N2 C18 1.481(5) . ?
C1 C2 1.485(7) . ?
C3 C4 1.446(8) . ?
C5 C6 1.378(8) . ?
C7 C8 1.470(7) . ?
C9 C10 1.389(6) . ?
C9 C14 1.405(6) . ?
C10 C11 1.343(8) . ?
C11 C12 1.379(8) . ?
C12 C13 1.382(7) . ?
C13 C14 1.384(6) . ?
C14 C15 1.439(6) . ?
C16 C17 1.514(6) . ?
C17 C18 1.507(6) . ?
C19 C20 1.413(6) . ?
C20 C21 1.393(5) . ?
C20 C25 1.397(6) . ?
C21 C22 1.385(6) . ?
C22 C23 1.377(6) . ?
C23 C24 1.383(7) . ?
C24 C25 1.358(7) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139135077
