Modular O- <i>vs.</i> N-coordination of pyridylidene amide ligands to iron determines activity in alcohol oxidation catalysis.
Verhoeven, Dide G. A.; Albrecht, Martin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17674–17682; doi:10.1039/d0dt02818e

data_7706190
_publ_section_title
;
 Modular O- <i>vs.</i> N-coordination of pyridylidene amide ligands to
 iron determines activity in alcohol oxidation catalysis.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17674
_journal_page_last               17682
_journal_paper_doi               10.1039/d0dt02818e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H22 Cl4 Fe2 N6 O2'
_chemical_formula_sum            'C24 H22 Cl4 Fe2 N6 O2'
_chemical_formula_weight         679.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                82.941(3)
_cell_angle_beta                 84.961(3)
_cell_angle_gamma                77.506(3)
_cell_formula_units_Z            1
_cell_length_a                   7.4259(3)
_cell_length_b                   8.5641(3)
_cell_length_c                   10.8957(4)
_cell_measurement_reflns_used    7837
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.7330
_cell_measurement_theta_min      1.8730
_cell_volume                     670.04(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_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    -16.00 112.00   1.00    4.00    --   27.42  77.00-150.00  128
  2  \w    -10.00 103.00   1.00    4.00    --   27.42  57.00   0.00  113
  3  \w     35.00 122.00   1.00    4.00    --   27.42 178.00   0.00   87
  4  \w    -10.00 103.00   1.00    4.00    --   27.42  57.00-180.00  113
  5  \w    -16.00 112.00   1.00    4.00    --   27.42  77.00  90.00  128
  6  \w     35.00 122.00   1.00    4.00    --   27.42 178.00  90.00   87
  7  \w    -54.00  83.00   1.00    4.00    --   27.42 -38.00 120.00  137
  8  \w    -16.00 112.00   1.00    4.00    --   27.42  77.00-120.00  128
  9  \w    -49.00  65.00   1.00    4.00    --   27.42 -57.00-120.00  114
 10  \w     35.00 122.00   1.00    4.00    --   27.42 178.00-150.00   87
 11  \w   -119.00 -64.00   1.00    4.00    --  -23.50 178.00 -90.00   55
 12  \w    -16.00 112.00   1.00    4.00    --   27.42  77.00   0.00  128
 13  \w     35.00 122.00   1.00    4.00    --   27.42 178.00 150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0143997000
_diffrn_orient_matrix_UB_12      -0.0436381000
_diffrn_orient_matrix_UB_13      0.0584175000
_diffrn_orient_matrix_UB_21      -0.0328792000
_diffrn_orient_matrix_UB_22      0.0733140000
_diffrn_orient_matrix_UB_23      0.0265090000
_diffrn_orient_matrix_UB_31      -0.0912218000
_diffrn_orient_matrix_UB_32      -0.0004723000
_diffrn_orient_matrix_UB_33      -0.0143105000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14261
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.119
_diffrn_reflns_theta_min         1.887
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.517
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       plate
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.5110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2691
_reflns_number_total             3046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02818e2.cif
_cod_data_source_block           19ma043_dv67
_cod_database_code               7706190
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C12 H11 Cl2 Fe I N3 O'
_chemical_oxdiff_usercomment     DV67
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              86065
_olex2_submission_special_instructions 'No special instructions were received'