Bis[μ-methylenebis(dicyclohexylphosphine)-<i>P</i>:<i>P</i>']bis[chloropalladium(I)](<i>Pd</i>—<i>Pd</i>) Diacetonitrile Solvate
Hashioka, Miho; Sakai, Ken; Tsubomura, Taro; Acta Crystallographica Section C 54 (1998) 1244–1247; doi:10.1107/S0108270198004521

data_2007660
_publ_section_title
;Bis[\m-methylenebis(dicyclohexylphosphine)-<i>P</i>:<i>P</i>']bis[chloropalladium(I)](<i>Pd</i>---<i>Pd</i>)
 Diacetonitrile Solvate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1244
_journal_page_last               1247
_journal_paper_doi               10.1107/S0108270198004521
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Pd2 Cl2 (C25 H46 P2)2].2C2 H3 N'
_chemical_formula_moiety         'Pd2 Cl2 P4 C50 H92,2(C2 H3 N)'
_chemical_formula_sum            'C54 H98 Cl2 N2 P4 Pd2'
_chemical_formula_weight         1183.0
_chemical_name_systematic
;
Bis[\m-methylenebis(dicyclohexylphosphine)-
P:P']bis[chloropalladium(I)](Pd---Pd)
Bis(acetonitrile) Solvate
;
_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_type_scat_source           IntTabC
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.44(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.021(5)
_cell_length_b                   17.118(4)
_cell_length_c                   12.110(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      28.74
_cell_volume                     5809(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;  MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1994a)
;
_computing_data_reduction
'PROCESS in TEXSAN (Molecular Structure Corporation, 1994b)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_sigmaI/netI    0.1110
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17784
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        3.8
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.031
_refine_ls_extinction_coef       0.00047(8)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         16865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.160
_refine_ls_R_factor_obs          .064
_refine_ls_shift/esd_max         0.029
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0410P)^2^+15.4P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.184
_refine_ls_wR_factor_obs         .121
_reflns_number_gt                9124
_reflns_number_total             16930
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            oa1051.cif
_cod_data_source_block           dcpm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value '\y scan' was replaced with
the value 'psi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2007660
_cod_database_fobs_code          2007660