Heteroligand Molecular "Stirrups" Using Conformationally Flexible Ditopic Pyridyl-Pyrazolyl Ligands
Jinzhen Lu; David R. Turner; Lindsay P. Harding; Stuart R. Batten; Inorganic Chemistry 48 (2009) 7525–7527; doi:10.1021/ic9010967

data_4302978
_publ_section_title
;
Heteroligand Molecular "Stirrups" Using Conformationally Flexible
Ditopic Pyridyl-Pyrazolyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7525
_journal_page_last               7527
_journal_paper_doi               10.1021/ic9010967
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C88 H80 N8 P4 Pd2, 4(C F3 O3 S)'
_chemical_formula_sum            'C92 H80 F12 N8 O12 P4 Pd2 S4'
_chemical_formula_weight         2182.56
_chemical_name_common            '[Pd2(dppp)2(4,4'-bipy)(LmXy)].4(OTf)'
_chemical_name_systematic
;
 [Pd2(dppp)2(4,4'-bipy)(LmXy)].4(OTf)
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.7475(8)
_cell_length_b                   13.1008(4)
_cell_length_c                   27.9322(9)
_cell_measurement_reflns_used    67263
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.28
_cell_volume                     11617.5(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1390
_diffrn_reflns_av_sigmaI/netI    0.1320
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            67263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.9509
_exptl_absorpt_correction_T_min  0.9052
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 Microanalytical data is consistent with refined molecular formulation.
 Electron density in void space is therefore assigned to volatile species.
;
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(0)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         19362
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2651
_reflns_number_gt                12236
_reflns_number_total             19362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9010967_si_002_1.cif
_cod_data_source_block           jl549b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Empirical' changed to 'empirical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4302978