Selective functionalization of C(sp3)–H bonds: catalytic chlorination and bromination by IronIII-acacen-halide under ambient condition
Shen, Chang; Dagnaw, Wasihun Menberu; Fong, Ching Wai; Lau, Kai Chung; Chow, Cheuk-Fai; Chemical Communications  (2022) –; doi:10.1039/D2CC02924C

data_7130684
_publ_section_title
;
 Selective functionalization of C(sp3)--H bonds: catalytic chlorination
 and bromination by IronIII-acacen-halide under ambient condition
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02924C
_journal_year                    2022
_chemical_formula_sum            'C12 H18 Br Fe N2 O2'
_chemical_formula_weight         358.04
_chemical_name_systematic        FeIII(acacen)(Br)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-07-24 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.458(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3529(16)
_cell_length_b                   24.649(5)
_cell_length_c                   8.2656(14)
_cell_measurement_reflns_used    196
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.64
_cell_volume                     1468.2(5)
_computing_cell_refinement       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_collection       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction        'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25004
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.926
_diffrn_reflns_theta_min         3.275
_exptl_absorpt_coefficient_mu    3.744
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2015)'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0407P)^2^+0.9209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2900
_reflns_number_total             3508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02924c2.cif
_cod_data_source_block           SCFe-2B
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130684
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.316
_shelx_estimated_absorpt_t_max   0.400
_shelx_res_checksum              97405
_shelx_hkl_checksum              92188