Stable Fe(iii) phenoxyimines as selective and robust CO<sub>2</sub>/epoxide coupling catalysts.
Fazekas, Eszter; Nichol, Gary S.; Shaver, Michael P.; Garden, Jennifer A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13106–13112; doi:10.1039/c8dt02919a

data_7047386
_publ_section_title
;
 Stable Fe(iii) phenoxyimines as selective and robust
 CO<sub>2</sub>/epoxide coupling catalysts.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13106
_journal_page_last               13112
_journal_paper_doi               10.1039/c8dt02919a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C16 H14 Cl3 Fe N2 O2'
_chemical_formula_sum            'C16 H14 Cl3 Fe N2 O2'
_chemical_formula_weight         428.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-13 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4166(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.1547(3)
_cell_length_b                   12.00241(14)
_cell_length_c                   12.99462(16)
_cell_measurement_reflns_used    13515
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.8080
_cell_measurement_theta_min      3.8950
_cell_volume                     3526.89(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -70.00  29.00   1.00    5.00    --  -41.92  65.00   1.00   99
  2  \w   -115.00 -19.00   1.00    5.00    --  -41.92 -38.00  90.00   96
  3  \w    -64.00  31.00   1.00    5.00    --  -41.92  38.00 -90.00   95
  4  \w     57.00 129.00   1.00    5.00    --   41.92 178.00-180.00   72
  5  \w     57.00 129.00   1.00    5.00    --   41.92 178.00 -60.00   72
  6  \w     36.00 135.00   1.00   20.00    --  111.00 -30.00 -90.00   99
  7  \w     41.00 139.00   1.00   20.00    --  111.00 -61.00 -60.00   98
  8  \w     87.00 178.00   1.00   20.00    --  111.00  30.00-180.00   91
  9  \w     94.00 178.00   1.00   20.00    --  111.00 125.00 -90.00   84
 10  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00 -30.00   79
 11  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00  60.00   79
 12  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00 120.00   79
 13  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00 -60.00   79
 14  \w     39.00 121.00   1.00   20.00    --  111.00-125.00  90.00   82
 15  \w     83.00 178.00   1.00   20.00    --  111.00  61.00-120.00   95
 16  \w     87.00 178.00   1.00   20.00    --  111.00  30.00-120.00   91
 17  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 -60.00   82
 18  \w     87.00 178.00   1.00   20.00    --  111.00  45.00  60.00   91
 19  \w     94.00 178.00   1.00   20.00    --  111.00 125.00-150.00   84
 20  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 -90.00   82
 21  \w     66.00 178.00   1.00   20.00    --  111.00  15.00-150.00  112
 22  \w     40.00 135.00   1.00   20.00    --  111.00 -45.00-180.00   95
 23  \w     39.00 121.00   1.00   20.00    --  111.00-125.00-150.00   82
 24  \w     94.00 178.00   1.00   20.00    --  111.00 125.00-120.00   84
 25  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00-150.00   79
 26  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 120.00   82
 27  \w     40.00  84.00   1.00   20.00    --  111.00-125.00   0.00   44
 28  \w    114.00 158.00   1.00   20.00    --  111.00 125.00 -30.00   44
 29  \w    105.00 150.00   1.00   20.00    --  111.00 125.00 120.00   45
 30  \w    102.00 131.00   1.00   20.00    --  111.00 -30.00-180.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0208322000
_diffrn_orient_matrix_UB_12      0.1081463000
_diffrn_orient_matrix_UB_13      0.0445053000
_diffrn_orient_matrix_UB_21      0.0466111000
_diffrn_orient_matrix_UB_22      -0.0164659000
_diffrn_orient_matrix_UB_23      0.1029783000
_diffrn_orient_matrix_UB_31      0.0451477000
_diffrn_orient_matrix_UB_32      0.0670778000
_diffrn_orient_matrix_UB_33      -0.0463543000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27812
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.025
_diffrn_reflns_theta_min         3.910
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.142
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_recrystallization_method
'The material was recrystallised from dichloromethane by slow evaporation'
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0790P)^2^+1.6030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3446
_reflns_number_total             3677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02919a2.cif
_cod_data_source_block           C3
_cod_depositor_comments
'Adding full bibliography for 7047385--7047387.cif.'
_cod_original_cell_volume        3526.89(7)
_cod_database_code               7047386
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H14 Cl3 Fe N2 O2'
_chemical_oxdiff_usercomment     '@ 120 K EFP88'
_shelx_estimated_absorpt_t_max   0.606
_shelx_estimated_absorpt_t_min   0.427
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              62133
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id EFP88
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.625