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_7123997
_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_absolute_configuration unk
_chemical_formula_sum            'C52.5 H49 Cl Fe O4'
_chemical_formula_weight         835.22
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-08-06 deposited with the CCDC.    2019-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4570(15)
_cell_length_b                   16.9138(18)
_cell_length_c                   17.4369(18)
_cell_measurement_reflns_used    7970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      1.68
_cell_volume                     4263.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0894
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55660
_diffrn_reflns_theta_full        27.20
_diffrn_reflns_theta_max         27.20
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.9338
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9380
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1041P)^2^+12.7949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2277
_refine_ls_wR_factor_ref         0.2324
_reflns_number_gt                7970
_reflns_number_total             9380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc05319k3.cif
_cod_data_source_block           sg772_0m
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C52.50 H49 Cl Fe O4'
_cod_database_code               7123997