#------------------------------------------------------------------------------
#$Date: 2022-06-24 02:18:55 +0300 (Fri, 24 Jun 2022) $
#$Revision: 276212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/05/7710587.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_7710587
loop_
_publ_author_name
'Yeung, Jason'
'Becker, Matthias'
'Stephan, Douglas W.'
_publ_section_title
;
 Towards macrocyclic frustrated Lewis pairs
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01716D
_journal_year                    2022
_chemical_formula_moiety         'C30 H28 B2 N2 O4'
_chemical_formula_sum            'C30 H28 B2 N2 O4'
_chemical_formula_weight         502.216
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                112.635(3)
_cell_angle_beta                 99.067(4)
_cell_angle_gamma                108.572(4)
_cell_formula_units_Z            1
_cell_length_a                   7.8349(13)
_cell_length_b                   9.0678(13)
_cell_length_c                   10.3304(16)
_cell_measurement_reflns_used    3708
_cell_measurement_temperature    149.49
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.68
_cell_volume                     608.31(17)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.49
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9929
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9929
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11686
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9929
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.9478.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             264.124
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.2864
_refine_diff_density_min         -0.2895
_refine_diff_density_rms         0.0585
_refine_ls_d_res_high            0.7795
_refine_ls_d_res_low             6.7531
_refine_ls_goodness_of_fit_ref   1.0584
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0584
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0430P)²+0.2015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -11
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2051
_reflns_number_total             2672
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt01716d2.cif
_cod_data_source_block           FINAL_a
_cod_database_code               7710587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C008(H00a,H00b), C00A(H00c,H00d)
2.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C009(H009), C00B(H00e), C00C(H00f), C00D(H00g), C00E(H00h),
 C00F(H00i), C00G(H00j), C00H(H00k), C00I(H00l)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -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_refinement_flags_posn
O001 O 0.45227(14) 0.39538(12) 0.09598(10) 0.0218(2) Uani 1.000000 .
O002 O 0.61888(15) 0.56857(12) 0.36029(10) 0.0248(2) Uani 1.000000 .
N003 N 0.75642(16) 0.66116(14) 0.18616(12) 0.0197(3) Uani 1.000000 .
C004 C 0.6462(2) 0.73409(18) 0.44284(15) 0.0218(3) Uani 1.000000 .
C005 C 0.7544(2) 0.37683(17) 0.19861(15) 0.0216(3) Uani 1.000000 .
C006 C 0.7328(2) 0.86635(18) 0.40486(16) 0.0230(3) Uani 1.000000 .
C007 C 0.7894(2) 0.82044(18) 0.27499(16) 0.0234(3) Uani 1.000000 .
H007 H 0.8543(2) 0.91147(18) 0.25317(16) 0.0280(4) Uiso 1.000000 R
C008 C 0.8276(2) 0.62933(19) 0.05824(16) 0.0236(3) Uani 1.000000 .
H00a H 0.9043(2) 0.74369(19) 0.06448(16) 0.0284(4) Uiso 1.000000 R
H00b H 0.9120(2) 0.56902(19) 0.06332(16) 0.0284(4) Uiso 1.000000 R
C009 C 0.6971(2) 0.21049(18) 0.08212(16) 0.0253(3) Uani 1.000000 .
H009 H 0.5806(2) 0.16139(18) 0.00524(16) 0.0303(4) Uiso 1.000000 R
C00A C 0.3302(2) 0.48073(18) 0.08910(15) 0.0221(3) Uani 1.000000 .
H00c H 0.2754(2) 0.49576(18) 0.17095(15) 0.0265(4) Uiso 1.000000 R
H00d H 0.4029(2) 0.59848(18) 0.09966(15) 0.0265(4) Uiso 1.000000 R
C00B C 0.9278(2) 0.44311(19) 0.30832(16) 0.0264(3) Uani 1.000000 .
H00e H 0.9711(2) 0.55624(19) 0.39015(16) 0.0316(4) Uiso 1.000000 R
C00C C 0.9780(2) 0.1840(2) 0.18385(18) 0.0287(4) Uani 1.000000 .
H00f H 1.0538(2) 0.1197(2) 0.17785(18) 0.0344(4) Uiso 1.000000 R
C00D C 0.7701(2) 1.04216(19) 0.49760(18) 0.0314(4) Uani 1.000000 .
H00g H 0.8288(2) 1.13119(19) 0.47175(18) 0.0377(4) Uiso 1.000000 R
C00E C 1.0388(2) 0.3488(2) 0.30154(18) 0.0299(4) Uani 1.000000 .
H00h H 1.1560(2) 0.3978(2) 0.37765(18) 0.0358(4) Uiso 1.000000 R
C00F C 0.5954(2) 0.7791(2) 0.57185(16) 0.0288(4) Uani 1.000000 .
H00i H 0.5349(2) 0.6912(2) 0.59833(16) 0.0346(4) Uiso 1.000000 R
C00G C 0.8054(2) 0.1129(2) 0.07429(17) 0.0299(4) Uani 1.000000 .
H00j H 0.7610(2) -0.0018(2) -0.00574(17) 0.0358(4) Uiso 1.000000 R
C00H C 0.7220(2) 1.0854(2) 0.62527(18) 0.0350(4) Uani 1.000000 .
H00k H 0.7485(2) 1.2042(2) 0.68838(18) 0.0421(5) Uiso 1.000000 R
C00I C 0.6345(2) 0.9542(2) 0.66118(17) 0.0347(4) Uani 1.000000 .
H00l H 0.6004(2) 0.9846(2) 0.74904(17) 0.0417(5) Uiso 1.000000 R
B00J B 0.6358(2) 0.4946(2) 0.20854(17) 0.0206(3) Uani 1.000000 .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
B 0.00141 0.00067 2.05450 1.33260 1.09790 0.70680 23.21850 1.02100 60.34980
0.14030 -0.193200007081
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
B00J O001 C00A 118.44(10) . . ?
B00J O002 C004 125.98(11) . . ?
C008 N003 C007 118.49(12) . . ?
B00J N003 C007 122.28(12) . . ?
B00J N003 C008 119.22(10) . . ?
C006 C004 O002 120.76(13) . . ?
C00F C004 O002 119.95(13) . . ?
C00F C004 C006 119.24(13) . . ?
C00B C005 C009 116.49(13) . . ?
B00J C005 C009 123.28(13) . . ?
B00J C005 C00B 120.19(12) . . ?
C007 C006 C004 119.01(12) . . ?
C00D C006 C004 120.04(14) . . ?
C00D C006 C007 120.89(14) . . ?
C006 C007 N003 123.00(13) . . ?
H007 C007 N003 118.50(8) . . ?
H007 C007 C006 118.50(8) . . ?
H00a C008 N003 108.98(7) . . ?
H00b C008 N003 108.98(7) . . ?
H00b C008 H00a 107.8 . . ?
C00A C008 N003 113.00(11) 2_665 . ?
C00A C008 H00a 108.98(7) 2_665 . ?
C00A C008 H00b 108.98(7) 2_665 . ?
H009 C009 C005 118.94(8) . . ?
C00G C009 C005 122.11(14) . . ?
C00G C009 H009 118.94(9) . . ?
C008 C00A O001 109.06(11) 2_665 . ?
H00c C00A O001 109.87(7) . . ?
H00c C00A C008 109.87(7) . 2_665 ?
H00d C00A O001 109.87(7) . . ?
H00d C00A C008 109.87(7) . 2_665 ?
H00d C00A H00c 108.3 . . ?
H00e C00B C005 118.87(8) . . ?
C00E C00B C005 122.25(14) . . ?
C00E C00B H00e 118.87(9) . . ?
C00E C00C H00f 120.18(9) . . ?
C00G C00C H00f 120.18(9) . . ?
C00G C00C C00E 119.65(13) . . ?
H00g C00D C006 119.85(10) . . ?
C00H C00D C006 120.29(15) . . ?
C00H C00D H00g 119.85(9) . . ?
C00C C00E C00B 119.73(14) . . ?
H00h C00E C00B 120.13(9) . . ?
H00h C00E C00C 120.13(9) . . ?
H00i C00F C004 120.38(9) . . ?
C00I C00F C004 119.24(15) . . ?
C00I C00F H00i 120.38(10) . . ?
C00C C00G C009 119.74(14) . . ?
H00j C00G C009 120.13(9) . . ?
H00j C00G C00C 120.13(9) . . ?
H00k C00H C00D 120.29(10) . . ?
C00I C00H C00D 119.41(14) . . ?
C00I C00H H00k 120.29(9) . . ?
C00H C00I C00F 121.76(15) . . ?
H00l C00I C00F 119.12(10) . . ?
H00l C00I C00H 119.12(9) . . ?
O002 B00J O001 111.61(12) . . ?
N003 B00J O001 109.16(11) . . ?
N003 B00J O002 106.75(10) . . ?
C005 B00J O001 111.38(11) . . ?
C005 B00J O002 109.51(11) . . ?
C005 B00J N003 108.27(11) . . ?
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
O001 C00A 1.4184(16) . ?
O001 B00J 1.4396(18) . ?
O002 C004 1.3336(16) . ?
O002 B00J 1.4958(18) . ?
N003 C007 1.2893(17) . ?
N003 C008 1.4770(18) . ?
N003 B00J 1.6298(19) . ?
C004 C006 1.407(2) . ?
C004 C00F 1.398(2) . ?
C005 C009 1.3879(19) . ?
C005 C00B 1.401(2) . ?
C005 B00J 1.610(2) . ?
C006 C007 1.430(2) . ?
C006 C00D 1.4086(19) . ?
C007 H007 0.9500 . ?
C008 H00a 0.9900 . ?
C008 H00b 0.9900 . ?
C008 C00A 1.514(2) 2_665 ?
C009 H009 0.9500 . ?
C009 C00G 1.398(2) . ?
C00A H00c 0.9900 . ?
C00A H00d 0.9900 . ?
C00B H00e 0.9500 . ?
C00B C00E 1.393(2) . ?
C00C H00f 0.9500 . ?
C00C C00E 1.380(2) . ?
C00C C00G 1.387(2) . ?
C00D H00g 0.9500 . ?
C00D C00H 1.374(2) . ?
C00E H00h 0.9500 . ?
C00F H00i 0.9500 . ?
C00F C00I 1.393(2) . ?
C00G H00j 0.9500 . ?
C00H H00k 0.9500 . ?
C00H C00I 1.387(3) . ?
C00I H00l 0.9500 . ?
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
O001 C00A C008 N003 -58.11(12) . . 2_665 2_665 ?
O001 B00J O002 C004 -101.44(12) . . . . ?
O001 B00J N003 C007 108.00(12) . . . . ?
O001 B00J N003 C008 -70.72(13) . . . . ?
O001 B00J C005 C009 9.26(15) . . . . ?
O001 B00J C005 C00B -172.94(11) . . . . ?
O002 C004 C006 C007 0.75(15) . . . . ?
O002 C004 C006 C00D -176.52(12) . . . . ?
O002 C004 C00F C00I 176.47(13) . . . . ?
O002 B00J N003 C007 -12.78(14) . . . . ?
O002 B00J N003 C008 168.50(10) . . . . ?
O002 B00J C005 C009 133.20(12) . . . . ?
O002 B00J C005 C00B -49.00(14) . . . . ?
N003 C007 C006 C004 3.53(16) . . . . ?
N003 C007 C006 C00D -179.23(13) . . . . ?
N003 B00J C005 C009 -110.76(12) . . . . ?
N003 B00J C005 C00B 67.04(13) . . . . ?
C004 C006 C00D C00H -0.09(16) . . . . ?
C004 C00F C00I C00H 0.25(17) . . . . ?
C005 C009 C00G C00C -1.45(18) . . . . ?
C005 C00B C00E C00C -0.23(18) . . . . ?
C006 C00D C00H C00I -0.71(17) . . . . ?
C009 C00G C00C C00E 1.65(18) . . . . ?
C00B C00E C00C C00G -0.84(18) . . . . ?
C00D C00H C00I C00F 0.64(17) . . . . ?
