Understanding Pd-Pd Bond Length Variation in (PNP)Pd-Pd(PNP) Dimers
Justin R. Walensky; Claudia M. Fafard; Chengyun Guo; Christina M. Brammell; Bruce M. Foxman; Michael B. Hall; Oleg V. Ozerov; Inorganic Chemistry 52 (2013) 2317–2322; doi:10.1021/ic301629m

data_4333966
_publ_section_title
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 Understanding Pd-Pd Bond Length Variation in (PNP)Pd-Pd(PNP) Dimers
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2317
_journal_page_last               2322
_journal_paper_doi               10.1021/ic301629m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C62 H100 N2 P4 Pd2'
_chemical_formula_sum            'C62 H100 N2 P4 Pd2'
_chemical_formula_weight         1210.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-01-08
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 95.8618(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5297(7)
_cell_length_b                   14.9059(6)
_cell_length_c                   21.7591(8)
_cell_measurement_reflns_used    9303
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     5978.5(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98551
_diffrn_reflns_theta_full        27.764
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         1.659
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.097
_refine_diff_density_max         1.94
_refine_diff_density_min         -2.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9882
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         14734
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.0156764
_refine_ls_shift/su_mean         0.0003527
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0698
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0698
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                11249
_reflns_number_total             14783
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0415
_oxford_refine_ls_scale          0.17081(3)
_oxford_reflns_number_all        14734
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ087_0m in P2(1)/c'
_cod_data_source_file            ic301629m_si_003.cif
_cod_data_source_block           oz087_final
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4333966
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, PD (1,U'S ) UNTIL C(62) 
CONT C(320,U[ISO]) C(321,U[ISO]) C(610,U[ISO]) UNTIL C(611) 
EQUIV C(610,OCC) C(611,OCC) H(6111,OCC) UNTIL H(6112) H(621,OCC) UNTIL H(623) 
CONT H(601,OCC) UNTIL H(602) H(6101,OCC) UNTIL H(6102) H(624,OCC) UNTIL H(626) 
CONT H(603,OCC) UNTIL H(604) 
EQUIV C(320,OCC) C(321,OCC) H(3211,OCC) H(3212,OCC) H(3213,OCC) 
CONT H(3201,OCC) H(3202,OCC) H(3203,OCC) 
WEIGHT -1.0  C(611,OCC) C(321,OCC) H(3211,OCC) H(3212,OCC) H(3213,OCC) 
WEIGHT -1.0  H(6111,OCC) UNTIL H(6112) H(621,OCC) UNTIL H(623) 
CONT H(601,OCC) UNTIL H(602) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H(302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
CONT H   ( 314,X'S) H   ( 315,X'S) H   ( 316,X'S) 
RIDE C   (  320,X'S) H   ( 3201,X'S) H   ( 3202,X'S) H   ( 3203,X'S) 
RIDE C   (  321,X'S) H   ( 3211,X'S) H   ( 3212,X'S) H   ( 3213,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) H   ( 493,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) H   ( 573,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) H   ( 583,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) H   ( 603,X'S) H   ( 604,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) H   ( 623,X'S) H   ( 624,X'S) 
CONT H   ( 625,X'S) H   ( 626,X'S) 
RIDE C   ( 610,X'S) H   (6101,X'S) H   (6102,X'S) 
RIDE C   ( 611,X'S) H   (6111,X'S) H   (6112,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.540000 , 0.015000 = C(54) TO C(55) 
END                                                                             
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