Synthesis and Reactions of the Homoleptic Chromium(II) Bis-amide [Ph2PN(iPr)P(Ph)N(iPr)−]2Cr with Relevance to a Selective Catalytic Ethene Trimerization System to 1-Hexene
Müller, Bernd H.; Peulecke, Normen; Spannenberg, Anke; Rosenthal, Uwe; Al-Hazmi, Mohammed H.; Schmidt, Roland; Wöhl, Anina; Müller, Wolfgang; Organometallics 31 (2012) 3695–; doi:10.1021/om300186a

data_4078274
_publ_section_title
;
 Synthesis and Reactions of the Homoleptic Chromium(II) Bis-amide
 [Ph2PN(iPr)P(Ph)N(iPr)&#x2212;]2Cr with Relevance to a Selective
 Catalytic Ethene Trimerization System to 1-Hexene
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3695
_journal_paper_doi               10.1021/om300186a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C62 H74 Cr N4 P4'
_chemical_formula_weight         1051.13
_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_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                 101.691(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9603(5)
_cell_length_b                   11.7532(2)
_cell_length_c                   24.2643(6)
_cell_measurement_reflns_used    5800
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      1.69
_cell_volume                     5574.3(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            92286
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.8995
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         13316
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0584P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                8137
_reflns_number_total             13316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300186a_si_001.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4078274