Heterobimetallic Al−Cl−Cr Intermediates with Relevance to the Selective Catalytic Ethene Trimerization Systems Consisting of CrCl3(THF)3, the Aminophosphorus Ligands Ph2PN(R)P(Ph)N(R)H, and Triethylaluminum
Peitz, Stephan; Peulecke, Normen; Müller, Bernd H.; Spannenberg, Anke; Drexler, Hans-Joachim; Rosenthal, Uwe; Al-Hazmi, Mohammed H.; Al-Eidan, Khalid E.; Wöhl, Anina; Müller, Wolfgang; Organometallics 30 (2011) 2364–; doi:10.1021/om200100g

data_4064431
_publ_section_title
;
 Heterobimetallic Al&#x2212;Cl&#x2212;Cr Intermediates with Relevance to
 the Selective Catalytic Ethene Trimerization Systems Consisting of
 CrCl3(THF)3, the Aminophosphorus Ligands Ph2PN(R)P(Ph)N(R)H, and
 Triethylaluminum
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2364
_journal_paper_doi               10.1021/om200100g
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C52 H70 Al2 Cl4 Cr2 N4 P4'
_chemical_formula_weight         1174.76
_chemical_name_systematic
; 
 ? 
;
_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                73.90(3)
_cell_angle_beta                 86.20(3)
_cell_angle_gamma                79.93(3)
_cell_formula_units_Z            2
_cell_length_a                   10.601(2)
_cell_length_b                   15.658(3)
_cell_length_c                   27.998(6)
_cell_measurement_reflns_used    29005
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      1.37
_cell_volume                     4395.6(17)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_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  0.0765
_diffrn_reflns_av_sigmaI/netI    0.1381
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47125
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.9165
_exptl_absorpt_correction_T_min  0.8159
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
The contribution of disordered solvent was taken into account using PLATON/SQUEEZE.
;
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         15463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0630P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                7070
_reflns_number_total             15463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200100g_si_002.cif
_cod_data_source_block           2d
_cod_original_cell_volume        4395.5(15)
_cod_database_code               4064431