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_7120764
_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_sum            'C118.5 H194.5 Cl11.5 N4 O56 Pd2'
_chemical_formula_weight         3191.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1j0k9d
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-05-13 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                   15.7481(2)
_cell_length_b                   31.2188(5)
_cell_length_c                   33.7366(4)
_cell_measurement_reflns_used    52314
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.9740
_cell_measurement_theta_min      3.8380
_cell_volume                     16586.2(4)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_molecular_graphics    'MERCURY 3.3(CCDC, 2014)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0662
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_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  0.1166
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            204136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.927
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.116
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       prism
_exptl_crystal_F_000             6676
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.088
_refine_diff_density_max         2.960
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.262
_refine_ls_abs_structure_details
;
 Flack x determined using 12019 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(4)
_refine_ls_extinction_coef       0.0024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.531
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1748
_refine_ls_number_reflns         31751
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.531
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.1236
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3477
_refine_ls_wR_factor_ref         0.3546
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                29211
_reflns_number_total             31751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06434a2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C118.50 H194.50 Cl11.50 N4 O56 Pd2'
_cod_database_code               7120764
_shelxl_version_number           2014/6
_shelx_res_checksum              71027