Heterobimetallic catechol-phosphine complexes with palladium and a group-13 element: structural flexibility and dynamics.
Bauer, G.; Nieger, M.; Gudat, D.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 8911–8920; doi:10.1039/c4dt00785a

data_7030475
_publ_section_title
;
 Heterobimetallic catechol-phosphine complexes with palladium and a
 group-13 element: structural flexibility and dynamics.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8911
_journal_page_last               8920
_journal_paper_doi               10.1039/c4dt00785a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C43 H37 Al O6 P2 Pd, 2(C H4 O)'
_chemical_formula_sum            'C45 H45 Al O8 P2 Pd'
_chemical_formula_weight         909.13
_chemical_name_systematic
; 
 Acetylacetonato-Bis-(mu-((diphenylphosphino)methyl)benzene-1,2-bis(olato))-A
luminium(III)-Palladium(II)
;
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.11(1)
_cell_angle_beta                 112.09(1)
_cell_angle_gamma                97.42(1)
_cell_formula_units_Z            2
_cell_length_a                   12.393(2)
_cell_length_b                   13.325(2)
_cell_length_c                   13.465(2)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2013.8(6)
_computing_cell_refinement       EVALCCD
_computing_data_collection       Collect
_computing_data_reduction        EVALCCD
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD    (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.1239
_diffrn_reflns_av_sigmaI/netI    0.1265
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28365
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABD (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
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_refine_diff_density_max         1.125
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0700P)^2^+7.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                4608
_reflns_number_total             7058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00785a2.cif
_cod_data_source_block           dg127_hy_compound_5
_cod_depositor_comments
;Adding full bibliography for 7030474--7030477.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_cell_volume        2013.8(5)
_cod_database_code               7030475