Controlled nitrite anion encapsulation and release in the molecular cavity of decamethylcucurbit[5]uril: solution and solid state studies
Lin, Jing-Xiang; Chen, Yu-Xi; Zhao, Dan; Chen, Yu; Lu, Xiu-Qiang; Lü, Jian; Cao, Rong; Inorganic Chemistry Frontiers 6 (2019) 303–; doi:10.1039/C8QI01168K

data_4349953
_publ_section_title
;
 Controlled nitrite anion encapsulation and release in the molecular
 cavity of decamethylcucurbit[5]uril: solution and solid state studies
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              303
_journal_paper_doi               10.1039/C8QI01168K
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C40 H50 N21 Na2 O14, 14.75(O), 0.5(N2 O4)'
_chemical_formula_sum            'C40 H50 N22 Na2 O30.75'
_chemical_formula_weight         1376.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_Int_Tables_number      13
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r1)
;
_audit_update_record
;
2017-12-13 deposited with the CCDC.
2018-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2140(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.98368(14)
_cell_length_b                   14.58477(15)
_cell_length_c                   19.3219(3)
_cell_measurement_reflns_used    16029
_cell_measurement_temperature    100.01(14)
_cell_measurement_theta_max      73.2960
_cell_measurement_theta_min      4.6210
_cell_volume                     3055.32(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9922
_diffrn_measured_fraction_theta_max 0.9911
_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   -119.00  -6.00   1.00    1.00    --  -40.15 -77.00  90.00  113
  2  \w    -95.00  -2.00   1.00    1.00    --  -40.15 125.00-150.00   93
  3  \w    -34.00  70.00   1.00    1.00    --   40.15 -57.00 -30.00  104
  4  \w     32.00 134.00   1.00    1.00    --  106.29 -45.00 -90.00  102
  5  \w     94.00 178.00   1.00    1.00    --  106.29 125.00   0.00   84
  6  \w     94.00 178.00   1.00    1.00    --  106.29 125.00  60.00   84
  7  \w     28.00 137.00   1.00    1.00    --  106.29 -30.00 -90.00  109
  8  \w     22.00 109.00   1.00    1.00    --  106.29 -94.00 120.00   87
  9  \w     22.00 109.00   1.00    1.00    --  106.29 -94.00  90.00   87
 10  \w     94.00 178.00   1.00    1.00    --  106.29 125.00  30.00   84
 11  \w    -67.00  36.00   1.00    1.00    --  -40.15  38.00-150.00  103
 12  \w   -114.00 -11.00   1.00    1.00    --  -40.15 -57.00 -60.00  103
 13  \w   -114.00 -11.00   1.00    1.00    --  -40.15 -57.00-180.00  103
 14  \w     76.00 178.00   1.00    1.00    --  106.29  30.00-180.00  102
 15  \w     45.00 178.00   1.00    1.00    --  106.29  15.00  90.00  133
 16  \w     32.00  84.00   1.00    1.00    --  106.29 -45.00  90.00   52
 17  \w     45.00 178.00   1.00    1.00    --  106.29  15.00 -30.00  133
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0746467000
_diffrn_orient_matrix_UB_12      0.0779074000
_diffrn_orient_matrix_UB_13      0.0271306000
_diffrn_orient_matrix_UB_21      -0.0547249000
_diffrn_orient_matrix_UB_22      -0.0687898000
_diffrn_orient_matrix_UB_23      0.0471823000
_diffrn_orient_matrix_UB_31      0.1077789000
_diffrn_orient_matrix_UB_32      0.0190091000
_diffrn_orient_matrix_UB_33      0.0596519000
_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  0.0231
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29606
_diffrn_reflns_theta_full        73.4051
_diffrn_reflns_theta_max         73.41
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1430.3757
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.6122
_refine_diff_density_min         -0.7574
_refine_diff_density_rms         0.1057
_refine_ls_d_res_high            0.8044
_refine_ls_d_res_low             11.5856
_refine_ls_goodness_of_fit_ref   1.0400
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0400
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0730
_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/[\s^2^(Fo^2^)+(0.1121P)^2^+7.7613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2049
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -10
_reflns_number_gt                5648
_reflns_number_total             6097
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8qi01168k2.cif
_cod_data_source_block           exp_21457
_cod_original_cell_volume        3055.32(6)
_cod_original_sg_symbol_Hall     '-P 2yc (x-z,y,z)'
_cod_database_code               4349953
_chemical_oxdiff_formula         'C40 H60 N20 O20 Na2'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O0aa(0.5) O1aa(0.5) O3aa(0.5) N5aa(0.5) O6aa(0.125) O1(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C29(H29a,H29b), C31(H31a,H31b), C36(H36a,H36b), C38(H38a,H38b), C40(H40a,H40b)
3.b Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C42(H42a,H42b,
 H42c), C43(H43a,H43b,H43c)
;
_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 1.948
_oxdiff_exptl_absorpt_empirical_full_min 0.602