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_4088094
_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            'C138 H156 B2 F30 Fe2 N6 O8'
_chemical_formula_weight         2730.01
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                79.366(5)
_cell_angle_beta                 71.927(5)
_cell_angle_gamma                77.544(5)
_cell_formula_units_Z            1
_cell_length_a                   14.380(5)
_cell_length_b                   15.676(5)
_cell_length_c                   17.063(5)
_cell_measurement_reflns_used    9545
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.71
_cell_measurement_theta_min      2.91
_cell_volume                     3542(2)
_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 0.948
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43597
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.13
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    2.456
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.078
_platon_squeeze_details
;
1 molecule of tetrahydrofuran solvate per asymmetric unit was treated
as a diffuse contribution to the overall scattering through the
use of platon/squeeze.
;
_refine_diff_density_max         1.061
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         11736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+4.3626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                10963
_reflns_number_total             11736
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00839_si_003.cif
_cod_data_source_block           bs20
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4088094