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_4302979
_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)(LpXy)].4(OTf)'
_chemical_name_systematic
;
 [p-xylene]
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 93.262(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.0643(8)
_cell_length_b                   23.5338(6)
_cell_length_c                   18.5747(6)
_cell_measurement_reflns_used    27210
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      1.10
_cell_volume                     12248.0(6)
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_collection       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27210
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.9269
_exptl_absorpt_correction_T_min  0.9182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
 Microanalytical results confirm that all electron density accounted for
 by SQUEEZE is from volatile species, i.e. solvent.
;
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0733
_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          0.2181
_refine_ls_wR_factor_ref         0.2433
_reflns_number_gt                5345
_reflns_number_total             8238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9010967_si_002_2.cif
_cod_data_source_block           jl526a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4302979