#------------------------------------------------------------------------------
#$Date: 2026-05-06 00:56:31 +0200 (Wed, 06 May 2026) $
#$Revision: 305876 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/72/09/7720987.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_7720987
loop_
_publ_author_name
'Li, Haowen'
'Wang, Xiao'
'Chai, Hui'
'Zhang, Fangfang'
_publ_section_title
;
 Design of borate-squarate hybrid crystals with large birefringence by
 synergistic assembly of planar π-conjugated groups.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d6dt00783j
_journal_year                    2026
_chemical_formula_moiety         '0.5(C4 H6 B2 O10 Rb2)'
_chemical_formula_sum            'C2 H3 B O5 Rb'
_chemical_formula_weight         203.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-03-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-03-05 deposited with the CCDC.	2026-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.365(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.591(2)
_cell_length_b                   7.3534(12)
_cell_length_c                   8.4758(16)
_cell_measurement_reflns_used    1869
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.88
_cell_volume                     603.35(19)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0682
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6805
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.878
_exptl_absorpt_coefficient_mu    8.150
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.7358.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0055(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         751
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0270
_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)+(0.0203P)²+0.6757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                585
_reflns_number_total             751
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00783j2.cif
_cod_data_source_block           Rb_3
_cod_original_cell_volume        603.36(19)
_cod_database_code               7720987
_shelx_shelxl_version_number     2019/3
_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   0.496
_shelx_estimated_absorpt_t_min   0.441
_olex2_refinement_description
;
1. Restrained distances
 O2-H2
 0.8 with sigma of 0.01
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
B1 B 0.1642(5) 0.500000 0.2638(6) 0.0313(11) Uani 1 2 d S T P . .
C1 C 0.6000(4) 0.500000 0.1172(5) 0.0269(9) Uani 1 2 d S T P . .
C2 C 0.4634(4) 0.500000 0.0862(5) 0.0279(9) Uani 1 2 d S T P . .
O1 O 0.0442(3) 0.500000 0.2560(4) 0.0370(8) Uani 1 2 d S T P . .
O2 O 0.1650(3) 0.500000 0.1039(4) 0.0449(9) Uani 1 2 d DS T P . .
O3 O 0.2877(3) 0.500000 0.4344(4) 0.0390(8) Uani 1 2 d S T P . .
O4 O 0.4202(3) 0.500000 0.1932(4) 0.0384(8) Uani 1 2 d S T P . .
O5 O 0.7220(3) 0.500000 0.2609(4) 0.0410(8) Uani 1 2 d S T P . .
Rb1 Rb 0.500000 0.75829(5) 0.500000 0.0390(2) Uani 1 2 d S T P . .
H1 H -0.021(5) 0.500000 0.157(7) 0.041(14) Uiso 1 2 d S . P . .
H2 H 0.241(2) 0.500000 0.125(7) 0.060(17) Uiso 1 2 d DS . P . .
H3 H 0.280(5) 0.500000 0.520(6) 0.047(15) Uiso 1 2 d S . P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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 121.4(4) . . ?
O1 B1 O3 120.1(4) . . ?
O1 B1 Rb1 139.31(18) . . ?
O1 B1 Rb1 139.31(18) . 5_666 ?
O2 B1 O3 118.6(4) . . ?
O2 B1 Rb1 87.6(2) . 5_666 ?
O2 B1 Rb1 87.6(2) . . ?
O3 B1 Rb1 42.46(13) . . ?
O3 B1 Rb1 42.46(13) . 5_666 ?
Rb1 B1 Rb1 60.55(7) 5_666 . ?
C2 C1 C2 89.7(3) . 5_665 ?
O5 C1 C2 135.4(3) . 5_665 ?
O5 C1 C2 134.9(3) . . ?
C1 C2 C1 90.3(3) . 5_665 ?
O4 C2 C1 135.5(3) . 5_665 ?
O4 C2 C1 134.2(3) . . ?
B1 O1 Rb1 122.01(19) . 7_566 ?
B1 O1 Rb1 122.01(19) . 3_445 ?
B1 O1 H1 115(3) . . ?
Rb1 O1 Rb1 73.30(6) 7_566 3_445 ?
Rb1 O1 H1 109(3) 7_566 . ?
Rb1 O1 H1 109(3) 3_445 . ?
B1 O2 H2 113(4) . . ?
B1 O3 Rb1 119.08(17) . 5_666 ?
B1 O3 Rb1 119.08(17) . . ?
B1 O3 H3 113(3) . . ?
Rb1 O3 Rb1 81.48(7) 5_666 . ?
Rb1 O3 H3 110(2) 5_666 . ?
Rb1 O3 H3 110(2) . . ?
C2 O4 Rb1 125.81(14) . 5_666 ?
C2 O4 Rb1 125.81(14) . . ?
Rb1 O4 Rb1 80.85(7) 5_666 . ?
C1 O5 Rb1 143.79(9) . 7_666 ?
C1 O5 Rb1 143.79(9) . 3_545 ?
Rb1 O5 Rb1 66.65(5) 7_666 3_545 ?
B1 Rb1 B1 119.45(7) . 5_666 ?
B1 Rb1 Rb1 59.72(4) 5_666 5_666 ?
B1 Rb1 Rb1 59.72(4) . 5_666 ?
B1 Rb1 H3 106.7(6) 5_666 . ?
B1 Rb1 H3 28.8(8) . . ?
O1 Rb1 B1 117.00(8) 7_566 5_666 ?
O1 Rb1 B1 117.00(8) 3 . ?
O1 Rb1 B1 98.51(8) 7_566 . ?
O1 Rb1 B1 98.50(8) 3 5_666 ?
O1 Rb1 O1 106.70(6) 7_566 3 ?
O1 Rb1 O5 74.32(7) 3 3_455 ?
O1 Rb1 O5 74.32(7) 7_566 7_666 ?
O1 Rb1 O5 67.32(7) 3 7_666 ?
O1 Rb1 O5 67.32(7) 7_566 3_455 ?
O1 Rb1 Rb1 126.65(3) 7_566 5_666 ?
O1 Rb1 Rb1 53.35(3) 3 5_676 ?
O1 Rb1 Rb1 126.65(3) 3 5_666 ?
O1 Rb1 Rb1 53.35(3) 7_566 5_676 ?
O1 Rb1 H3 145.3(8) 3 . ?
O1 Rb1 H3 82.7(6) 7_566 . ?
O3 Rb1 B1 106.89(6) 5_666 . ?
O3 Rb1 B1 18.46(7) . . ?
O3 Rb1 B1 106.89(6) . 5_666 ?
O3 Rb1 B1 18.46(7) 5_666 5_666 ?
O3 Rb1 O1 135.03(8) 5_666 7_566 ?
O3 Rb1 O1 135.03(8) . 3 ?
O3 Rb1 O1 94.11(6) 5_666 3 ?
O3 Rb1 O1 94.11(7) . 7_566 ?
O3 Rb1 O3 98.52(7) 5_666 . ?
O3 Rb1 O4 64.37(7) . 5_666 ?
O3 Rb1 O4 65.55(7) 5_666 5_666 ?
O3 Rb1 O4 64.37(7) 5_666 . ?
O3 Rb1 O4 65.55(7) . . ?
O3 Rb1 O5 157.61(8) 5_666 3_455 ?
O3 Rb1 O5 157.61(7) . 7_666 ?
O3 Rb1 O5 78.02(5) . 3_455 ?
O3 Rb1 O5 78.02(5) 5_666 7_666 ?
O3 Rb1 Rb1 49.26(4) . 5_666 ?
O3 Rb1 Rb1 130.74(4) . 5_676 ?
O3 Rb1 Rb1 130.74(4) 5_666 5_676 ?
O3 Rb1 Rb1 49.26(4) 5_666 5_666 ?
O3 Rb1 H3 102.3(5) 5_666 . ?
O3 Rb1 H3 12.9(7) . . ?
O4 Rb1 B1 82.79(7) . 5_666 ?
O4 Rb1 B1 82.79(7) 5_666 . ?
O4 Rb1 B1 58.11(8) . . ?
O4 Rb1 B1 58.11(8) 5_666 5_666 ?
O4 Rb1 O1 155.89(8) 5_666 3 ?
O4 Rb1 O1 155.89(8) . 7_566 ?
O4 Rb1 O1 82.04(5) . 3 ?
O4 Rb1 O1 82.04(5) 5_666 7_566 ?
O4 Rb1 O4 99.15(7) 5_666 . ?
O4 Rb1 O5 94.63(6) . 3_455 ?
O4 Rb1 O5 129.18(7) 5_666 3_455 ?
O4 Rb1 O5 129.18(7) . 7_666 ?
O4 Rb1 O5 94.63(6) 5_666 7_666 ?
O4 Rb1 Rb1 130.43(3) 5_666 5_676 ?
O4 Rb1 Rb1 49.57(3) . 5_666 ?
O4 Rb1 Rb1 130.43(3) . 5_676 ?
O4 Rb1 Rb1 49.57(3) 5_666 5_666 ?
O4 Rb1 H3 78.1(6) . . ?
O4 Rb1 H3 56.6(7) 5_666 . ?
O5 Rb1 B1 172.68(8) 7_666 . ?
O5 Rb1 B1 64.03(5) 3_455 . ?
O5 Rb1 B1 64.03(5) 7_666 5_666 ?
O5 Rb1 B1 172.68(8) 3_455 5_666 ?
O5 Rb1 O5 113.35(5) 7_666 3_455 ?
O5 Rb1 Rb1 123.32(3) 3_455 5_666 ?
O5 Rb1 Rb1 56.68(3) 7_666 5_676 ?
O5 Rb1 Rb1 123.32(3) 7_666 5_666 ?
O5 Rb1 Rb1 56.68(3) 3_455 5_676 ?
O5 Rb1 H3 79.3(6) 3_455 . ?
O5 Rb1 H3 145.7(8) 7_666 . ?
Rb1 Rb1 B1 120.28(4) 5_676 . ?
Rb1 Rb1 B1 120.28(4) 5_676 5_666 ?
Rb1 Rb1 Rb1 180.0 5_676 5_666 ?
Rb1 Rb1 H3 125.7(5) 5_676 . ?
Rb1 Rb1 H3 54.3(5) 5_666 . ?
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 1.356(5) . ?
B1 O2 1.361(5) . ?
B1 O3 1.365(5) . ?
B1 Rb1 3.767(4) . ?
B1 Rb1 3.767(4) 5_666 ?
C1 C2 1.455(5) . ?
C1 C2 1.455(5) 5_665 ?
C1 O5 1.261(4) . ?
C2 O4 1.255(4) . ?
O1 Rb1 2.977(2) 3_445 ?
O1 Rb1 2.977(2) 7_566 ?
O1 H1 0.76(5) . ?
O2 H2 0.794(10) . ?
O3 Rb1 2.910(2) 5_666 ?
O3 Rb1 2.910(2) . ?
O3 H3 0.78(4) . ?
O4 Rb1 2.9289(19) 5_666 ?
O4 Rb1 2.9289(19) . ?
O5 Rb1 3.235(2) 7_666 ?
O5 Rb1 3.235(2) 3_545 ?
Rb1 Rb1 3.7987(10) 5_666 ?
Rb1 Rb1 3.5547(10) 5_676 ?
Rb1 H3 3.26(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 O4 Rb1 -53.09(15) . . . 5_666 ?
C1 C2 O4 Rb1 -126.91(15) 5_665 . . . ?
C1 C2 O4 Rb1 53.09(15) . . . . ?
C1 C2 O4 Rb1 126.91(15) 5_665 . . 5_666 ?
C2 C1 C2 C1 0.000(0) 5_665 . . 5_665 ?
C2 C1 C2 O4 180.000(0) 5_665 . . . ?
C2 C1 O5 Rb1 -111.6(3) . . . 7_666 ?
C2 C1 O5 Rb1 111.6(3) . . . 3_545 ?
C2 C1 O5 Rb1 68.4(3) 5_665 . . 7_666 ?
C2 C1 O5 Rb1 -68.4(3) 5_665 . . 3_545 ?
O1 B1 O3 Rb1 -131.69(13) . . . . ?
O1 B1 O3 Rb1 131.69(13) . . . 5_666 ?
O2 B1 O1 Rb1 135.25(13) . . . 3_445 ?
O2 B1 O1 Rb1 -135.25(14) . . . 7_566 ?
O2 B1 O3 Rb1 48.31(13) . . . . ?
O2 B1 O3 Rb1 -48.31(13) . . . 5_666 ?
O3 B1 O1 Rb1 -44.75(14) . . . 3_445 ?
O3 B1 O1 Rb1 44.75(14) . . . 7_566 ?
O5 C1 C2 C1 180.000(0) . . . 5_665 ?
O5 C1 C2 O4 0.000(1) . . . . ?
Rb1 B1 O1 Rb1 5.9(4) 5_666 . . 3_445 ?
Rb1 B1 O1 Rb1 -95.40(17) . . . 3_445 ?
Rb1 B1 O1 Rb1 95.40(17) 5_666 . . 7_566 ?
Rb1 B1 O1 Rb1 -5.9(4) . . . 7_566 ?
Rb1 B1 O3 Rb1 96.6(3) 5_666 . . . ?
Rb1 B1 O3 Rb1 -96.6(3) . . . 5_666 ?
