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_7047387
_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         '2(C24 H32 Cl Fe N2 O2), C7 H8'
_chemical_formula_sum            'C55 H72 Cl2 Fe2 N4 O4'
_chemical_formula_weight         1035.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.003(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8856(3)
_cell_length_b                   24.3385(7)
_cell_length_c                   19.8618(6)
_cell_measurement_reflns_used    7950
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.7930
_cell_measurement_theta_min      4.8330
_cell_volume                     5261.4(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_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 0.992
_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    -64.00  31.00   1.00    5.00    --  -41.67  38.00 -30.00   95
  2  \w   -114.00 -19.00   1.00    5.00    --  -41.67 -38.00-180.00   95
  3  \w   -127.00 -34.00   1.00    5.00    --  -41.67 178.00  30.00   93
  4  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00 120.00   79
  5  \w     37.00 142.00   1.00   20.00    --  111.00 -77.00-180.00  105
  6  \w     39.00 121.00   1.00   20.00    --  111.00-125.00 -60.00   82
  7  \w     36.00 135.00   1.00   20.00    --  111.00 -30.00 120.00   99
  8  \w     39.00 121.00   1.00   20.00    --  111.00-125.00-120.00   82
  9  \w     66.00 178.00   1.00   20.00    --  111.00  15.00  60.00  112
 10  \w     30.00 109.00   1.00   20.00    --  111.00 -94.00 -30.00   79
 11  \w     36.00 135.00   1.00   20.00    --  111.00 -30.00-120.00   99
 12  \w     93.00 135.00   1.00   20.00    --  111.00 -45.00 -60.00   42
 13  \w     69.00  98.00   1.00   20.00    --  111.00-118.00 128.00   29
 14  \w     34.00 102.00   1.00   20.00    --  111.00 -94.00  30.00   68
 15  \w     31.00  74.00   1.00   20.00    --  111.00 -94.00  60.00   43
 16  \w     88.00 142.00   1.00   20.00    --  111.00  30.00 120.00   54
 17  \w     45.00  80.00   1.00   20.00    --  111.00 -94.00 -60.00   35
;
_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      -0.0141350000
_diffrn_orient_matrix_UB_12      0.0620140000
_diffrn_orient_matrix_UB_13      0.0131211000
_diffrn_orient_matrix_UB_21      0.0370425000
_diffrn_orient_matrix_UB_22      -0.0088237000
_diffrn_orient_matrix_UB_23      0.0744324000
_diffrn_orient_matrix_UB_31      0.1359277000
_diffrn_orient_matrix_UB_32      0.0089194000
_diffrn_orient_matrix_UB_33      -0.0175151000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            10913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.021
_diffrn_reflns_theta_min         3.632
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.731
_exptl_absorpt_correction_T_max  0.4716
_exptl_absorpt_correction_T_min  0.2522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1197 before and 0.0935 after correction. The Ratio of minimum to maximum transmission is 0.5348. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       plate
_exptl_crystal_F_000             2192
_exptl_crystal_recrystallization_method
'The material was recrystallised from toluene by slow evaporation'
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0969
_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^)+(0.1005P)^2^+21.7650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7797
_reflns_number_total             10913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02919a2.cif
_cod_data_source_block           C2
_cod_depositor_comments
'Adding full bibliography for 7047385--7047387.cif.'
_cod_original_cell_volume        5261.3(3)
_cod_database_code               7047387
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H32 Cl Fe N2 O2'
_chemical_oxdiff_usercomment     '@ 120 K EFP213'
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.179
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.863(4)
 0.137(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C15(H15), C16(H16), C17(H17), C19(H19),
 C27(H27), C28(H28), C29(H29), C31(H31), C39(H39), C40(H40), C41(H41), C43(H43),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              94608
_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_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 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.702