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_7047385
_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 H16 Cl Fe N2 O2'
_chemical_formula_sum            'C16 H16 Cl Fe N2 O2'
_chemical_formula_weight         359.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 108.536(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5989(3)
_cell_length_b                   7.39494(17)
_cell_length_c                   17.7897(5)
_cell_measurement_reflns_used    10338
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.4980
_cell_measurement_theta_min      4.3470
_cell_volume                     1571.45(7)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.958
_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    -59.00  -4.00   1.00    5.00    --  -17.68 102.00  34.00   55
  2  \w    -12.00  93.00   1.00    5.00    --   19.09  77.00 -60.00  105
  3  \w    -12.00  93.00   1.00    5.00    --   19.09  77.00-150.00  105
  4  \w     -3.00  92.00   1.00    5.00    --   19.09  38.00-150.00   95
  5  \w    -20.00  59.00   1.00    5.00    --   19.09 -99.00  30.00   79
  6  \w     -3.00  92.00   1.00    5.00    --   19.09  38.00 120.00   95
  7  \w   -104.00 -57.00   1.00    5.00    --  -17.68-178.00 150.00   47
  8  \w    -51.00  46.00   1.00    5.00    --   19.09 -57.00-180.00   97
  9  \w     35.00  83.00   1.00    5.00    --   19.09 178.00-180.00   48
 10  \w    -20.00  59.00   1.00    5.00    --   19.09 -99.00-180.00   79
;
_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      -0.0366194000
_diffrn_orient_matrix_UB_12      -0.0190969000
_diffrn_orient_matrix_UB_13      -0.0386078000
_diffrn_orient_matrix_UB_21      -0.0051627000
_diffrn_orient_matrix_UB_22      -0.0905690000
_diffrn_orient_matrix_UB_23      0.0115280000
_diffrn_orient_matrix_UB_31      -0.0464408000
_diffrn_orient_matrix_UB_32      0.0251827000
_diffrn_orient_matrix_UB_33      0.0120646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.888
_diffrn_reflns_theta_min         3.008
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.413
_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    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_recrystallization_method
'The material was recrystallised from dichloromethane by slow evaporation'
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.217
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0263P)^2^+1.5933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2618
_reflns_number_total             2808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02919a2.cif
_cod_data_source_block           C1
_cod_depositor_comments
'Adding full bibliography for 7047385--7047387.cif.'
_cod_original_cell_volume        1571.44(7)
_cod_database_code               7047385
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C17 H17 Cl Fe N2 O2'
_chemical_oxdiff_usercomment     '@ 120 K EFP112'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              23169
_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 1.342
_oxdiff_exptl_absorpt_empirical_full_min 0.825