Palladium(ii)-directed formation of pseudo-rotaxanes : the 3 + 1 approach to threaded species using square-planar geometries
Hamann, C.; Kern, J.-M.; Sauvage, J.-P.; Dalton Transactions  (2003) 3770–; doi:10.1039/b306277e

data_7013291
_publ_section_title
;
 Palladium(ii)-directed formation of pseudo-rotaxanes : the 3 + 1
 approach to threaded species using square-planar geometries
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3770
_journal_paper_doi               10.1039/b306277e
_journal_year                    2003
_chemical_formula_moiety         'C94 H115 B4 F16 N9 O10 Pd2'
_chemical_formula_sum            'C94 H115 B4 F16 N9 O10 Pd2'
_chemical_formula_weight         2091.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                101.281(5)
_cell_angle_beta                 90.583(5)
_cell_angle_gamma                102.957(5)
_cell_formula_units_Z            2
_cell_length_a                   13.1827(2)
_cell_length_b                   18.5474(2)
_cell_length_c                   20.6953(4)
_cell_measurement_temperature    173
_cell_volume                     4828.25(19)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
21436 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  2.0 deg 1 scans of   60 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  101 frames
Set 2 Theta =   -6.30 Kappa = -152.00 Phi   =    0.00   28 frames
Friedel pairs were averaged. Internal R = 0.03
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21436
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9626
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.44
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.476
_refine_diff_density_min         -0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   25.708
_refine_ls_goodness_of_fit_ref   1.316
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1216
_refine_ls_number_reflns         13539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.089
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/esd_mean        0.002
_refine_ls_shift/su_max          0.022
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         1.199
_refine_ls_wR_factor_ref         0.073
_reflns_number_gt                13539
_reflns_number_total             21436
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b306277e.txt
_cod_data_source_block           st1065
_cod_original_cell_volume        4828.2(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013291