Synthesis and Electronic Structure of Iron Borate Betaine Complexes as a Route to Single-Component Iron Ethylene Oligomerization and Polymerization Catalysts
Schaefer, Brian A.; Margulieux, Grant W.; Tiedemann, Margaret A.; Small, Brooke L.; Chirik, Paul J.; Organometallics 34 (2015) 5615–; doi:10.1021/acs.organomet.5b00839

data_4088093
_publ_section_title
;
 Synthesis and Electronic Structure of Iron Borate Betaine Complexes as a
 Route to Single-Component Iron Ethylene Oligomerization and
 Polymerization Catalysts
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5615
_journal_paper_doi               10.1021/acs.organomet.5b00839
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C78 H77 Fe N4 P2'
_chemical_formula_weight         1188.23
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.112(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3168(12)
_cell_length_b                   14.8689(9)
_cell_length_c                   24.9609(14)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.61
_cell_measurement_theta_min      6.23
_cell_volume                     7034.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41395
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.5773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.053
_platon_squeeze_details
;
The asymmetric unit contained one molecule of disordered pentane
solvate which was treated as a diffuse contribution to the overall
scattering through the use of PLATON/SQUEEZE.
;
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         12004
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+3.1713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                9341
_reflns_number_total             12004
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00839_si_003.cif
_cod_data_source_block           bs18
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4088093