Photoresponsive Macrocycles for Selective Binding and Release of Sulfate
Xiong, Shenglun; He, Qing; Chemical Communications  (2021) –; doi:10.1039/D1CC05506B

data_7129271
_publ_section_title
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 Photoresponsive Macrocycles for Selective Binding and Release of Sulfate
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05506B
_journal_year                    2021
_chemical_formula_moiety         '2(C33 H30 N6 O4)'
_chemical_formula_sum            'C66 H60 N12 O8'
_chemical_formula_weight         1149.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-28 deposited with the CCDC.	2021-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.499(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3970(2)
_cell_length_b                   15.8981(4)
_cell_length_c                   50.4387(15)
_cell_measurement_reflns_used    3371
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      5.30
_cell_volume                     7528.1(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            52172
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.133
_diffrn_reflns_theta_max         67.133
_diffrn_reflns_theta_min         1.753
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1476 before and 0.0635 after correction.
The Ratio of minimum to maximum transmission is 0.8491.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00127(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         13304
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+8.9677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10073
_reflns_number_total             13304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05506b2.cif
_cod_data_source_block           2-trans
_cod_database_code               7129271
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C02S-C02O
 1.37 with sigma of 0.01
 N01Z-N02A \\sim N01{-N02A
 with sigma of 0.02
 N02A-N01{ \\sim N02B-N01{
 with sigma of 0.02
 N01Z-C02C \\sim N01{-C02C
 with sigma of 0.02
 N02A-C02N \\sim N02B-C02N
 with sigma of 0.02
 N01Z-N02A \\sim N01Z-N02B
 with sigma of 0.02
 C02R-N02B \\sim C02S-N02B
 with sigma of 0.02
 C02N-C02R \\sim C02N-C02S
 with sigma of 0.02
 C02N-C02P \\sim C02O-C02P
 with sigma of 0.02
 N02A-C02N \\sim N02A-C02O
 with sigma of 0.02
 C02N-C02S \\sim C02O-C02S
 with sigma of 0.02
 C02N-C02R \\sim C02O-C02R
 with sigma of 0.02
 C02N-N02B \\sim C02O-N02B
 with sigma of 0.02
 C02L-C02R \\sim C02L-C02S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N01{) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C02R) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C02O) \\sim Ueq, Uanis(C02N) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C02R) \\sim Ueq, Uanis(C02S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(N01{)=1-FVAR(1)
 Sof(N01Z)=FVAR(1)
 Sof(N02B)=1-FVAR(2)
 Sof(N02A)=FVAR(2)
 Sof(H02A)=Sof(C02S)=Sof(H02S)=1-FVAR(3)
 Sof(H02L)=Sof(C02R)=Sof(H02R)=FVAR(3)
 Sof(H02B)=Sof(C02O)=1-FVAR(4)
 Sof(C02N)=Sof(H02P)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C015(H01A,H01B), C019(H01C,H01D), C01E(H01G,H01H), C01F(H01P,H01Q), C01J(H01S,
 H01U), C01L(H01J,H01L), C01N(H01N,H01O), C01O(H01V,H01W), C01Q(H01Y,H),
 C01Y(H3,HA)
5.b Aromatic/amide H refined with riding coordinates:
 N009(H009), N00A(H00A), N00B(H00B), N00C(H00C), N00D(H00D), N00E(H00E),
 N00F(H00F), N00G(H00G), C00R(H00R), C010(H010), C014(H014), C018(H018),
 C01A(H01E), C01D(H01F), C01H(H01R), C01I(H01I), C01K(H01K), C01M(H01M),
 C01P(H01X), C01R(H01Z), C01S(H01), C01T(H01T), C01W(H1), C01X(H2), C020(H020),
 C021(H021), C023(H023), C024(H024), C026(H026), C027(H027), C029(H029),
 C02B(H02C), C02E(H02E), C02F(H02F), C02G(H02G), C02I(H02I), C02J(H02J),
 C02L(H02L), C02L(H02A), C02P(H02P), C02P(H02B), C02R(H02R), C02S(H02S)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64587
_shelx_fab_checksum              10560
_olex2_submission_special_instructions 'No special instructions were received'