Solvent- and anion-induced interconversions of metal-organic cages.
Li, Yu-Hao; Jiang, Ji-Jun; Fan, Yan-Zhong; Wei, Zhang-Wen; Chen, Cheng-Xia; Yu, Hui-Juan; Zheng, Shao-Ping; Fenske, Dieter; Su, Cheng-Yong; Barboiu, Mihail; Chemical communications (Cambridge, England) 52 (2016) 8745–8748; doi:10.1039/c6cc04420d

data_7124756
_publ_section_title
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 Solvent- and anion-induced interconversions of metal-organic cages.
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_journal_issue                   56
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8745
_journal_page_last               8748
_journal_paper_doi               10.1039/c6cc04420d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C106 H74.5 B3.5 F13.88 I0.5 N21 O4 Pd2'
_chemical_formula_weight         2284.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
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2016-03-12 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 125.0860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.9184(7)
_cell_length_b                   20.7337(3)
_cell_length_c                   28.9827(4)
_cell_measurement_reflns_used    14160
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.9890
_cell_measurement_theta_min      3.5040
_cell_volume                     21104.1(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            31255
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        62.499
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         3.507
_exptl_absorpt_coefficient_mu    4.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48167
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       bar
_exptl_crystal_F_000             9203
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1475
_refine_ls_number_reflns         16562
_refine_ls_number_restraints     557
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+51.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12904
_reflns_number_total             16562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04420d2.cif
_cod_data_source_block           Cage-I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C106 H74.50 B3.50 F13.88 I0.50 N21 O4 Pd2'
_cod_database_code               7124756
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.390
_shelx_estimated_absorpt_t_max   0.543
_exptl_absorpt_special_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

BF4- anions in the cage cavity were partially replaced by I-
anion, and the fractional ratio between these two anions
was freely refined as a result of about 50%.

Some acetontrile and BF4- molecules are disreded and refined
with partial occupancy and restrains for idealized model.
;
_shelx_res_checksum              66275
_shelx_hkl_checksum              84642