A new system for cyclohexane functionalization employing iron(III) catalysts and trichloroisocianuric acid
Gomes, Clicia; Lube, Leonardo Munaldi; Fernandes, Christiane; Franco, Roberto W. A.; Lamounier Camargos Resende, Jackson Antonio; Horn, Adolfo; New J. Chem. 41 (2017) 11498–11502; doi:10.1039/C7NJ01164D

data_7056475
_publ_section_title
;
 A new system for cyclohexane functionalization employing iron(III)
 catalysts and trichloroisocianuric acid
;
_journal_issue                   20
_journal_name_full               'New J. Chem.'
_journal_page_first              11498
_journal_page_last               11502
_journal_paper_doi               10.1039/C7NJ01164D
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C16 H18 Cl3 Fe N2 O2, C2 H3 N, 0.5(H2 O)'
_chemical_formula_sum            'C18 H21.75 Cl3 Fe N3 O2.5'
_chemical_formula_weight         482.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-12-04T00:28:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-05-27 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7516(16)
_cell_length_b                   28.169(2)
_cell_length_c                   7.3729(6)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.85
_cell_volume                     4309.8(6)
_computing_cell_refinement       'APEX2 (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Photon 100 detector'
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            37930
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.443
_diffrn_reflns_theta_min         2.438
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
        wR2(int) was 0.1020 before and 0.0544 after correction.
        The Ratio of minimum to maximum transmission is 0.7521.
        The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1982
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.66
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.1213
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+103.7580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2878
_refine_ls_wR_factor_ref         0.2983
_reflns_number_gt                3123
_reflns_number_total             4039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01164d2.cif
_cod_data_source_block           mo_c2814_0ma
_cod_original_formula_sum        'C18 H21.75 Cl3 Fe N3 O2.50'
_cod_database_code               7056475
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.937