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_7030476
_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         'C76 H61 Al O8 P4 Pd2, 2(C H2 Cl2)'
_chemical_formula_sum            'C78 H65 Al Cl4 O8 P4 Pd2'
_chemical_formula_weight         1635.76
_chemical_name_systematic
; 
 Tris-(mu-((diphenylphosphino)methyl)benzene-1,2-bis(olato)-(mu-((diphenylpho
sphino)methyl)-6-hydroxyphenolato)-aluminium(III)-dipalladium(II)
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.15(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.608(2)
_cell_length_b                   13.568(1)
_cell_length_c                   13.497(1)
_cell_measurement_reflns_used    281
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     3716.4(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1912
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6509
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.7985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
 4 solvent CH2Cl2 per unit cell
;
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6509
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                4126
_reflns_number_total             6509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00785a2.cif
_cod_data_source_block           dg128_sq_compound_6
_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        3716.4(5)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7030476