#------------------------------------------------------------------------------
#$Date: 2022-01-12 01:29:47 +0200 (Wed, 12 Jan 2022) $
#$Revision: 271992 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/41/7244187.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_7244187
loop_
_publ_author_name
'Chen, Chong-An'
'Yang, Guo-Yu'
_publ_section_title
;
 Syntheses, Structures and Optical Properties of Two B3O7 Cluster-based
 Borates
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01579F
_journal_year                    2022
_chemical_formula_sum            'C3 H14 B6 N2 O11'
_chemical_formula_weight         319.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-14 deposited with the CCDC.	2022-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.159(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5687(6)
_cell_length_b                   15.4864(11)
_cell_length_c                   9.0230(8)
_cell_measurement_reflns_used    2683
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3060
_cell_measurement_theta_min      4.5400
_cell_volume                     1194.18(16)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8014
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.429
_exptl_absorpt_coefficient_mu    0.161
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0602P)²+0.2661P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1741
_reflns_number_total             2101
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01579f2.cif
_cod_data_source_block           A1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7244187
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
B6 B 0.4652(2) 0.07759(13) 0.8213(2) 0.0155(4) Uani 1 1 d . . . . .
O8 O 0.35462(14) 0.13994(8) 0.81647(15) 0.0206(3) Uani 1 1 d . . . . .
O1 O -0.38052(13) 0.09405(8) 0.81992(14) 0.0179(3) Uani 1 1 d . . . . .
O4 O -0.13906(13) 0.16197(8) 0.79622(13) 0.0162(3) Uani 1 1 d . . . . .
O6 O 0.10649(13) 0.16564(8) 0.69587(14) 0.0193(3) Uani 1 1 d . . . . .
O7 O 0.14417(14) 0.16449(8) 0.96559(15) 0.0206(3) Uani 1 1 d . . . . .
H1 H 0.051647 0.178480 0.957428 0.031 Uiso 1 1 calc R U . . .
O5 O -0.11322(13) 0.21715(9) 0.55169(14) 0.0198(3) Uani 1 1 d . . . . .
O3 O -0.36582(13) 0.21172(9) 0.64630(14) 0.0183(3) Uani 1 1 d . . . . .
O2 O -0.34606(14) 0.24124(8) 0.90471(14) 0.0193(3) Uani 1 1 d . . . . .
O10 O 0.15215(14) 0.03144(8) 0.82858(15) 0.0199(3) Uani 1 1 d . . . . .
O9 O 0.41989(14) -0.00893(8) 0.81936(16) 0.0235(3) Uani 1 1 d . . . . .
O11 O 0.21311(16) -0.11164(9) 0.78796(18) 0.0312(4) Uani 1 1 d . . . . .
H2 H 0.287840 -0.142095 0.770368 0.047 Uiso 1 1 calc R U . . .
B3 B -0.0494(2) 0.18179(13) 0.6832(2) 0.0143(4) Uani 1 1 d . . . . .
B2 B -0.2736(2) 0.23080(13) 0.5340(2) 0.0148(4) Uani 1 1 d . . . . .
B1 B -0.3069(2) 0.17867(13) 0.7922(2) 0.0135(4) Uani 1 1 d . . . . .
B4 B 0.1870(2) 0.12534(13) 0.8266(2) 0.0168(5) Uani 1 1 d . . . . .
B5 B 0.2627(2) -0.02945(14) 0.8138(2) 0.0185(5) Uani 1 1 d . . . . .
N1 N 0.15650(18) 0.04035(10) 0.18881(17) 0.0208(4) Uani 1 1 d . . . . .
H1A H 0.157768 0.079815 0.117204 0.031 Uiso 1 1 calc R U . . .
H1B H 0.064302 0.013628 0.182899 0.031 Uiso 1 1 calc R U . . .
H1C H 0.232166 0.001956 0.178199 0.031 Uiso 1 1 calc R U . . .
N2 N 0.34316(19) 0.19639(11) 0.46798(19) 0.0253(4) Uani 1 1 d . . . . .
H2A H 0.262584 0.232193 0.473795 0.038 Uiso 1 1 calc R U . . .
H2B H 0.430973 0.226815 0.464839 0.038 Uiso 1 1 calc R U . . .
H2C H 0.350273 0.162032 0.547255 0.038 Uiso 1 1 calc R U . . .
C1 C 0.3192(3) 0.14320(15) 0.3312(3) 0.0337(5) Uani 1 1 d . . . . .
H1D H 0.412874 0.109590 0.318820 0.040 Uiso 1 1 calc R U . . .
H1E H 0.302673 0.181048 0.245888 0.040 Uiso 1 1 calc R U . . .
C2 C 0.1820(2) 0.08327(13) 0.3362(2) 0.0264(5) Uani 1 1 d . . . . .
H3 H 0.088641 0.116529 0.356527 0.032 Uiso 1 1 calc R U . . .
C3 C 0.2106(4) 0.01417(16) 0.4541(3) 0.0501(7) Uani 1 1 d . . . . .
H3A H 0.127913 -0.027742 0.444482 0.075 Uiso 1 1 calc R U . . .
H3B H 0.213017 0.040183 0.550830 0.075 Uiso 1 1 calc R U . . .
H3C H 0.308854 -0.013679 0.441671 0.075 Uiso 1 1 calc R 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'
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 B6 O8 123.42(17) 1_655 . ?
O1 B6 O9 117.00(16) 1_655 . ?
O8 B6 O9 119.49(16) . . ?
B6 O8 B4 125.22(15) . . ?
B6 O1 B1 126.74(14) 1_455 . ?
B3 O4 B1 123.55(14) . . ?
B3 O6 B4 123.42(14) . . ?
B3 O5 B2 119.04(14) . . ?
B2 O3 B1 124.25(14) . . ?
B2 O2 B1 134.27(14) 4_566 . ?
B5 O10 B4 122.66(14) . . ?
B5 O9 B6 119.42(15) . . ?
O4 B3 O6 120.24(17) . . ?
O4 B3 O5 121.64(16) . . ?
O6 B3 O5 118.11(16) . . ?
O2 B2 O3 117.17(16) 4_565 . ?
O2 B2 O5 122.45(16) 4_565 . ?
O3 B2 O5 120.29(17) . . ?
O4 B1 O2 112.11(15) . . ?
O4 B1 O3 110.99(14) . . ?
O2 B1 O3 108.10(14) . . ?
O4 B1 O1 105.65(14) . . ?
O2 B1 O1 110.33(14) . . ?
O3 B1 O1 109.66(14) . . ?
O8 B4 O6 106.93(15) . . ?
O8 B4 O7 107.33(15) . . ?
O6 B4 O7 112.43(15) . . ?
O8 B4 O10 110.55(14) . . ?
O6 B4 O10 110.12(15) . . ?
O7 B4 O10 109.42(15) . . ?
O10 B5 O11 117.29(17) . . ?
O10 B5 O9 121.69(17) . . ?
O11 B5 O9 120.98(17) . . ?
N2 C1 C2 112.29(17) . . ?
N1 C2 C1 108.29(16) . . ?
N1 C2 C3 108.51(17) . . ?
C1 C2 C3 111.8(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
B6 O1 1.347(2) 1_655 ?
B6 O8 1.351(2) . ?
B6 O9 1.395(2) . ?
O8 B4 1.464(2) . ?
O1 B1 1.483(2) . ?
O4 B3 1.356(2) . ?
O4 B1 1.459(2) . ?
O6 B3 1.356(2) . ?
O6 B4 1.463(3) . ?
O7 B4 1.463(2) . ?
O5 B3 1.383(2) . ?
O5 B2 1.388(2) . ?
O3 B2 1.362(2) . ?
O3 B1 1.468(2) . ?
O2 B2 1.352(2) 4_566 ?
O2 B1 1.460(2) . ?
O10 B5 1.350(2) . ?
O10 B4 1.485(2) . ?
O9 B5 1.381(2) . ?
O11 B5 1.357(3) . ?
N1 C2 1.489(2) . ?
N2 C1 1.485(3) . ?
C1 C2 1.501(3) . ?
C2 C3 1.516(3) . ?
