N-Phosphanyl- andN,N′-Diphosphanyl-Substituted N-Heterocyclic Carbene Chromium Complexes: Synthesis, Structures, and Catalytic Ethylene Oligomerization
Ai, Pengfei; Danopoulos, Andreas A.; Braunstein, Pierre; Organometallics 34 (2015) 4109–; doi:10.1021/acs.organomet.5b00547

data_4086185
_publ_section_title
;
 N-Phosphanyl- andN,N&#x2032;-Diphosphanyl-Substituted N-Heterocyclic
 Carbene Chromium Complexes: Synthesis, Structures, and Catalytic Ethylene
 Oligomerization
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4109
_journal_paper_doi               10.1021/acs.organomet.5b00547
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         '2(C40 H62 Cl2 Cr N4 P2), C4 H8 O'
_chemical_formula_sum            'C84 H132 Cl4 Cr2 N8 O P4'
_chemical_formula_weight         1639.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_cell_angle_alpha                92.3890(10)
_cell_angle_beta                 107.0430(10)
_cell_angle_gamma                103.6190(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8371(2)
_cell_length_b                   19.4080(5)
_cell_length_c                   20.7508(4)
_cell_measurement_reflns_used    46707
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     4769.68(17)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48574
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         1.034
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
The residual electron density was assigned to one molecule of the
tetrahydrofuran solvent [88/2 = 44 e per asymmetric unit; one molecule
of C4H8O1 would give 40 e]. 
;
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         21701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+1.8800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17364
_reflns_number_total             21701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00547_si_002.cif
_cod_data_source_block           pbad121203
_cod_depositor_comments
'Adding full bibliography for 4086184--4086189.cif.'
_cod_database_code               4086185
_shelxl_version_number           2013-4
_shelx_res_checksum              29597
_shelx_hkl_checksum              18525