Synthesis and coordinative properties of a hybrid bis(diphenylphosphino)methane‒terpyridine
Pickaert, Guillaume; Douce, Laurent; Ziessel, Raymond; Cesario, Michèle; Chemical Communications  (2000) 1125–; doi:10.1039/b002586k

data_7110957
_publ_section_title
;
 Synthesis and coordinative properties of a hybrid
 bis(diphenylphosphino)methane--terpyridine
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1125
_journal_paper_doi               10.1039/b002586k
_journal_year                    2000
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'Pd(C40 N3 P2 H30)'
_chemical_formula_sum            'C80 H60 N6 P4 Pd'
_chemical_formula_weight         1335.62
_chemical_name_common
'Bis(diphenylphosphino)methane-terpyridyl Pd complex'
_chemical_name_systematic
'Bis(diphenylphosphino)methane-terpyridyl Pd(II) complex'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.54(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.477(4)
_cell_length_b                   25.327(9)
_cell_length_c                   11.595(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3333(2)
_computing_cell_refinement       'HKL package (Otwinovski & Minor, 1997)'
_computing_data_collection       'Nonius Kappa-CCD Software'
_computing_data_reduction        'HKL package'
_computing_molecular_graphics    OrtepII
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius kappaCCD diffractometer'
_diffrn_measurement_method       'area-detector 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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27387
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+4.2395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1423
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                4185
_reflns_number_total             6772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002586ksup1.cif
_cod_data_source_block           ComplexPd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+4.2395P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+4.2395P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3333.1(22)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'Pd C80 N6 P4 H60 '
_cod_database_code               7110957