Aza-capped cyclodextrins for intra-cavity metal complexation
Sechet, D.; Kaya, Z.; Phan, T.-A.; Jouffroy, M.; Bentouhami, E.; Armspach, D.; Matt, D.; Toupet, L.; Chem. Commun.  (2017) –; doi:10.1039/C7CC06434A

data_7120765
_publ_section_title
;
 Aza-capped cyclodextrins for intra-cavity metal complexation
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06434A
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C67 H112 Cl2 N2 O33 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C69 H116 Cl6 N2 O33 Pd'
_chemical_formula_weight         1820.73
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-04-26 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.2881(8)
_cell_length_b                   29.3527(8)
_cell_length_c                   10.8184(3)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.05
_cell_measurement_theta_min      3.01
_cell_volume                     8982.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            68400
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.918
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'Cu-ImuS microfocus tube'
_exptl_absorpt_coefficient_mu    3.976
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       needle
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
The residual electron density was assigned one molecule of the pentane solvent [134/4= 34 e per asymmetric unit; one molecule of C5H12 would give 42 e].
;
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 3870 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.018(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         15613
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                11401
_reflns_number_total             15613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06434a2.cif
_cod_data_source_block           dazk170221
_cod_database_code               7120765
_shelx_estimated_absorpt_t_min   0.475
_shelx_estimated_absorpt_t_max   0.742
_shelxl_version_number           2013-4
_shelx_res_checksum              9826