Tying the alkoxides together: an iron complex of a new chelating bulky bis(alkoxide) demonstrates selectivity for coupling of non-bulky aryl nitrenes
Groysman, Stanislav; Lord, Richard L.; Wannipurage, Duleeka; Kurup, Sudheer S.; Chemical Communications  (2019) –; doi:10.1039/C9CC05319K

data_7123996
_publ_section_title
;
 Tying the alkoxides together: an iron complex of a new chelating bulky
 bis(alkoxide) demonstrates selectivity for coupling of non-bulky aryl
 nitrenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05319K
_journal_year                    2019
_chemical_formula_sum            'C22 H17 O'
_chemical_formula_weight         297.36
_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_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-97
_audit_update_record
;
2019-07-08 deposited with the CCDC.    2019-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                95.974(4)
_cell_angle_beta                 112.253(4)
_cell_angle_gamma                102.680(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5806(7)
_cell_length_b                   10.2480(8)
_cell_length_c                   10.6149(8)
_cell_measurement_reflns_used    1640
_cell_measurement_temperature    569(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.08
_cell_volume                     824.51(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex2'
_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  0.0992
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33851
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.9858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             314
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.138
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                1640
_reflns_number_total             3583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc05319k3.cif
_cod_data_source_block           sg827_0m
_cod_original_cell_volume        824.51(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7123996