Coexistence of 1 : 1 and 2 : 1 inclusion complexes of indigo carmine
Yanshyna, Oksana; Avram, Liat; Shimon, Linda J. W.; Klajn, Rafal; Chemical Communications  (2022) –; doi:10.1039/D1CC07081A

data_7129602
_publ_section_title
;
 Coexistence of 1&#x2009;:&#x2009;1 and 2&#x2009;:&#x2009;1 inclusion
 complexes of indigo carmine
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07081A
_journal_year                    2022
_chemical_formula_sum            'C256 H320 N88 O93 Pd12 S8'
_chemical_formula_weight         7651.26
_chemical_name_common            'indigo carmine'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2021-12-15 deposited with the CCDC.	2022-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                78.3060(10)
_cell_angle_beta                 82.3820(10)
_cell_angle_gamma                82.0000(10)
_cell_formula_units_Z            1
_cell_length_a                   18.5972(2)
_cell_length_b                   20.7368(3)
_cell_length_c                   30.3057(3)
_cell_measurement_reflns_used    141549
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.7850
_cell_measurement_theta_min      3.4450
_cell_volume                     11267.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.111a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 Dolomanov(2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            296248
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.154
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    4.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.111a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       plate
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.583
_refine_diff_density_min         -2.152
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2116
_refine_ls_number_reflns         45350
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1056P)^2^+20.9124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38815
_reflns_number_total             45350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07081a2.cif
_cod_data_source_block           22c1_2
_cod_database_code               7129602
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.603
_shelx_estimated_absorpt_t_max   0.912
_oxdiff_exptl_absorpt_empirical_full_min 0.582
_oxdiff_exptl_absorpt_empirical_full_max 1.605
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              3852
_shelx_fab_checksum              55342