Photo–Controllable Binding and Release of HP2O73– Using an Azobenzene based Smart Macrocycle
Xiong, Shenglun; Zhang, Yi; Jiang, Yunqi; Wang, Fei; Zhou, Wei; Li, Aimin; Zhang, Qinpeng; Wang, Qiuan; He, Qing; Chemical Communications  (2023) –; doi:10.1039/D3CC03608A

data_7132162
_publ_section_title
;
 Photo--Controllable Binding and Release of HP2O73-- Using an Azobenzene
 based Smart Macrocycle
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03608A
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C28 H32 N6 O2, C3 H7 N O'
_chemical_formula_sum            'C31 H39 N7 O3'
_chemical_formula_weight         557.70
_chemical_name_systematic        1-trans
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-07 deposited with the CCDC.	2023-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2849(2)
_cell_length_b                   14.4216(2)
_cell_length_c                   16.5790(2)
_cell_measurement_reflns_used    11867
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2050
_cell_measurement_theta_min      4.0490
_cell_volume                     2937.27(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9947
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     79.00 104.00   0.50    0.30    --  111.82  77.00 -30.00   50
  2  \w     80.00 165.00   0.50    0.30    --  111.82  30.00-120.00  170
  3  \w    143.00 169.00   0.50    0.30    --  111.82  77.00 -30.00   52
  4  \w    121.00 173.00   0.50    0.30    --  111.82  30.00  30.00  104
  5  \w     97.00 172.00   0.50    0.30    --  111.82  40.00 110.00  150
  6  \w    115.00 141.00   0.50    0.30    --  111.82  82.00 -73.00   52
  7  \w    -16.00  36.00   0.50    0.08    --   39.45 -40.00 -43.00  104
  8  \w    -30.00  18.00   0.50    0.08    --   39.45 -19.00  60.00   96
  9  \w     41.00 103.00   0.50    0.30    --  111.82 -77.00  60.00  124
 10  \w     41.00  68.00   0.50    0.30    --  111.82 -61.00 -30.00   54
 11  \w     41.00  99.00   0.50    0.30    --  111.82 -77.00 -90.00  116
 12  \w     47.00 103.00   0.50    0.30    --  111.82 -77.00-180.00  112
 13  \w     38.00  86.00   0.50    0.30    --  111.82 -77.00-120.00   96
 14  \w     38.00  68.00   0.50    0.30    --  111.82 -61.00 -90.00   60
 15  \w     43.00  68.00   0.50    0.30    --  111.82 -61.00 -60.00   50
 16  \w     38.00  67.00   0.50    0.30    --  111.82 -61.00  90.00   58
 17  \w     40.00  67.00   0.50    0.30    --  111.82 -61.00  60.00   54
 18  \w     72.00 101.00   0.50    0.30    --  111.82-149.00 -70.00   58
 19  \w     64.00  97.00   0.50    0.30    --  111.82-111.00 -60.00   66
 20  \w     36.00  74.00   0.50    0.30    --  111.82-123.00  92.00   76
 21  \w   -119.00 -93.00   0.50    0.30    --  -52.00 -94.00  90.00   52
 22  \w   -114.00 -83.00   0.50    0.30    --  -52.00-123.00  92.00   62
 23  \w   -126.00 -71.00   0.50    0.30    --  -52.00-149.00 -70.00  110
 24  \w     -8.00  23.00   0.50    0.30    --  -52.00  15.00 -90.00   62
 25  \w    -75.00  30.00   0.50    0.08    --  -39.45  82.00 -73.00  210
 26  \w    104.00 129.00   0.50    0.30    --  111.82  40.00 110.00   50
 27  \w     38.00  63.00   0.50    0.30    --  111.82 -61.00   0.00   50
 28  \w     38.00  63.00   0.50    0.30    --  111.82 -61.00-150.00   50
 29  \w     -6.00  20.00   0.50    0.08    --   39.45 -82.00 164.00   52
 30  \w     85.00 111.00   0.50    0.30    --  111.82 111.00 -90.00   52
 31  \w     -5.00  20.00   0.50    0.08    --   39.45 -82.00 164.00   50
 32  \w    -44.00 -19.00   0.50    0.08    --  -39.45  82.00 -73.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0764139000
_diffrn_orient_matrix_UB_12      0.0447433000
_diffrn_orient_matrix_UB_13      -0.0625761000
_diffrn_orient_matrix_UB_21      0.0778760000
_diffrn_orient_matrix_UB_22      0.0296461000
_diffrn_orient_matrix_UB_23      0.0681092000
_diffrn_orient_matrix_UB_31      0.0619226000
_diffrn_orient_matrix_UB_32      -0.0923738000
_diffrn_orient_matrix_UB_33      -0.0084464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9947
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19146
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9836
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.71
_diffrn_reflns_theta_min         4.06
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             1186.851
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.3418
_refine_diff_density_min         -0.3529
_refine_diff_density_rms         0.0397
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.13(10)
_refine_ls_d_res_high            0.7955
_refine_ls_d_res_low             10.8810
_refine_ls_goodness_of_fit_ref   1.0494
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0494
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.4818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.969
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                5628
_reflns_number_total             6009
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc03608a2.cif
_cod_data_source_block           3045-X4-100K_autored
_cod_depositor_comments
;

2025-03-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C9.538 H12 N2.154 O0.923'
_cod_original_formula_weight         172.208
_cod_original_formula_moiety         '0.308(C28 H32 N6 O2), 0.308(C3 H7 N O)'
_cod_original_formula_units_Z            13
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7132162
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C010(H01a,H01b), C013(H01c,H01d)
2.b Aromatic/amide H refined with riding coordinates:
 N005(H005), C00C(H00C), C00G(H00G), C00I(H00I), C00L(H00L), C00M(H00M),
 C00O(H00O), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z),
 C011(H011), C012(H012)
2.c Idealised Me refined as rotating group:
 C00N(H00a,H00b,H00d), C00S(H00e,H00f,H00h), C00T(H00j,H00k,H00n), C00Y(H00p,
 H00q,H00r), C014(H01e,H01f,H01g), C015(H01h,H01i,H01j)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.639