Di-μ-chlorido-bis{[μ-1,8-bis(diisopropylphosphanyl)-9,10-dihydro-9,10-ethanoanthracene-κ^2^<i>P</i>:<i>P</i>']-μ-chlorido-μ-methylidene-dipalladium(II)} tetrahydrofuran pentasolvate
Schnetz, Thomas; Rominger, Frank; Hofmann, Peter; Acta Crystallographica Section E 66 (2010) m453–m454; doi:10.1107/S1600536810010263

data_2225541
_publ_section_title
;
 Di-\m-chlorido-bis{[\m-1,8-bis(diisopropylphosphanyl)-9,10-dihydro-9,10-ethanoanthracene-\k^2^<i>P</i>:<i>P</i>']-\m-chlorido-\m-methylidene-dipalladium(II)}
 tetrahydrofuran pentasolvate
;
_journal_coeditor_code           HG2653
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m453
_journal_page_last               m454
_journal_paper_doi               10.1107/S1600536810010263
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pd4 (C H2)2 Cl4 (C28 H40 P2)2], 5C4 H8 O'
_chemical_formula_moiety         'C58 H84 Cl4 P4 Pd4, 5(C4 H8 O)'
_chemical_formula_sum            'C78 H124 Cl4 O5 P4 Pd4'
_chemical_formula_weight         1833.05
_chemical_name_systematic
;
Di-\m-chlorido-bis{[\m-1,8-bis(diisopropylphosphanyl)-9,10-dihydro-
9,10-ethanoanthracene-\k^2^<i>P</i>:<i>P</i>']-\m-chlorido-\m-methylidene-
dipalladium(II)} tetrahydrofuran pentasolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.8770(10)
_cell_angle_beta                 74.7030(10)
_cell_angle_gamma                80.7170(10)
_cell_formula_units_Z            2
_cell_length_a                   12.57990(10)
_cell_length_b                   17.2830(3)
_cell_length_c                   19.7558(2)
_cell_measurement_reflns_used    5889
_cell_measurement_temperature    200(2)
_cell_volume                     4048.61(9)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008b)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w 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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36611
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.9351
_exptl_absorpt_correction_T_min  0.8221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008a)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.727
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         15292
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.8053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                9483
_reflns_number_total             15292
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg2653.cif
_cod_data_source_block           I
_cod_database_code               2225541
_cod_database_fobs_code          2225541