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_7132161
_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'
_chemical_formula_sum            'C28 H32 N6 O2'
_chemical_formula_weight         480.574
_chemical_name_systematic        1-cis
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_symmetry_Int_Tables_number      41
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-11 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                   11.4339(5)
_cell_length_b                   9.3891(4)
_cell_length_c                   24.5636(11)
_cell_measurement_reflns_used    1835
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7240
_cell_measurement_theta_min      10.1030
_cell_volume                     2637.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9845
_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    -39.00  -9.00   1.00    1.00    --    0.00 113.00-148.00   30
  2  \w      8.00  51.00   1.00    1.63    --   54.00 -69.00-161.00   43
  3  \w     58.00  84.00   1.00    1.63    --   54.00  54.00 135.00   26
  4  \w    124.00 174.00   1.00    1.63    --  108.00  69.00 -29.00   50
  5  \w     88.00 156.00   1.00    1.63    --  108.00  54.00 135.00   68
  6  \w     75.00 100.00   1.00    1.63    --  108.00 -69.00-161.00   25
  7  \w    101.00 126.00   1.00    1.63    --  108.00 -54.00  -8.00   25
  8  \w     39.00  94.00   1.00    1.63    --  108.00-113.00 119.00   55
  9  \w      2.00  35.00   1.00    1.00    --    0.00  77.00   0.00   33
 10  \w     58.00  84.00   1.00    1.63    --   54.00-125.00-180.00   26
 11  \w      7.00  96.00   1.00    1.63    --   54.00 -99.00   0.00   89
 12  \w     29.00  56.00   1.00    1.63    --   54.00  37.00 150.00   27
 13  \w    100.00 125.00   1.00    1.63    --   54.00  37.00 150.00   25
 14  \w    106.00 178.00   1.00    1.63    --  108.00  77.00   0.00   72
 15  \w     36.00 109.00   1.00    1.63    --  108.00-111.00-180.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0598477000
_diffrn_orient_matrix_UB_12      0.0476660000
_diffrn_orient_matrix_UB_13      0.0104217000
_diffrn_orient_matrix_UB_21      -0.0152151000
_diffrn_orient_matrix_UB_22      0.0956132000
_diffrn_orient_matrix_UB_23      0.1043143000
_diffrn_orient_matrix_UB_31      0.0111673000
_diffrn_orient_matrix_UB_32      -0.1247936000
_diffrn_orient_matrix_UB_33      0.0842678000
_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  0.0172
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9845
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            3578
_diffrn_reflns_point_group_measured_fraction_full 0.7145
_diffrn_reflns_point_group_measured_fraction_max 0.6984
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         70.52
_diffrn_reflns_theta_min         3.60
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             1019.352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.1055
_refine_diff_density_min         -0.1437
_refine_diff_density_rms         0.0290
_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   0.01(18)
_refine_ls_d_res_high            0.8177
_refine_ls_d_res_low             12.2818
_refine_ls_goodness_of_fit_ref   1.0647
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    29
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1760
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0647
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.397
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              29
_reflns_limit_l_min              -29
_reflns_number_gt                1676
_reflns_number_total             1760
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc03608a2.cif
_cod_data_source_block           exp_524
_cod_original_sg_symbol_Hall     ' A 2 -2ab'
_cod_database_code               7132161
_chemical_oxdiff_formula         'C1 H1 N1 O1 Cl1'
_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:
 C00D(H00a,H00d)
2.b Aromatic/amide H refined with riding coordinates:
 N002(H002), N003(H003), C007(H007), C00B(H00B), C00C(H00C), C00F(H00h),
 C00G(H00i), C00I(H00m), C00J(H00n)
2.c Idealised Me refined as rotating group:
 C00E(H00e,H00f,H00g), C00H(H00j,H00k,H00l)
;
_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 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.771