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_4086188
_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         'C44 H58 Cr N2 P'
_chemical_formula_sum            'C44 H58 Cr N2 P'
_chemical_formula_weight         697.89
_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                80.3450(10)
_cell_angle_beta                 78.2590(10)
_cell_angle_gamma                72.6140(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0437(3)
_cell_length_b                   13.3177(4)
_cell_length_c                   16.8347(6)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.31
_cell_volume                     2090.14(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34586
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.083
_diffrn_reflns_theta_min         1.613
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       prism
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_platon_squeeze_details
;
 The residual electron density was assigned to half a molecule of the
 pentane solvent [42/2 = 21 e per asymmetric unit; half a molecule of
 C5H12 would give 21e]. 
;
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         12219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0520P)^2^+0.1286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9642
_reflns_number_total             12219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00547_si_002.cif
_cod_data_source_block           shelx6
_cod_depositor_comments
'Adding full bibliography for 4086184--4086189.cif.'
_cod_database_code               4086188
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2013-4
_shelx_res_checksum              22775
_shelx_hkl_checksum              10168