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_7706191
_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         'C19 H17 Cl2 Fe N5 O2, 2(C2 H6 O S)'
_chemical_formula_sum            'C23 H29 Cl2 Fe N5 O4 S2'
_chemical_formula_weight         630.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-19
_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                90
_cell_angle_beta                 93.6941(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.80925(5)
_cell_length_b                   18.68619(9)
_cell_length_c                   9.50696(5)
_cell_measurement_reflns_used    11929
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      77.2430
_cell_measurement_theta_min      4.6520
_cell_volume                     1384.422(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (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 10.0000
_diffrn_detector_type            HyPix
_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    -92.00  -5.00   0.50    0.25    --  -18.75 -32.00   8.00  174
  2  \w    -31.00  56.00   0.50    0.25    --  -18.75  32.00 167.00  174
  3  \w    -25.00  34.00   0.50    0.25    --   47.95 -32.00   8.00  118
  4  \w     35.00 122.00   0.50    0.25    --   47.95  32.00 167.00  174
  5  \w     95.00 174.00   0.50    1.00    --  107.75  32.00 167.00  158
  6  \w    -66.00  -9.00   0.50    0.25    --  -18.75 125.00-180.00  114
  7  \w    -26.00  23.00   0.50    0.25    --   47.95 -19.00-150.00   98
  8  \w     35.00 109.00   0.50    1.00    --  107.75 -94.00 120.00  148
  9  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00 -60.00   66
 10  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00-150.00   66
 11  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00  60.00   66
 12  \w     35.00 102.00   0.50    1.00    --  107.75 -77.00-120.00  134
 13  \w     92.00 174.00   0.50    1.00    --  107.75  61.00-180.00  164
 14  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00  90.00   66
 15  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00 150.00   66
 16  \w     35.00 109.00   0.50    1.00    --  107.75 -94.00  60.00  148
 17  \w     35.00 109.00   0.50    1.00    --  107.75 -94.00 150.00  148
 18  \w     35.00 102.00   0.50    1.00    --  107.75 -77.00-150.00  134
 19  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00   0.00   66
 20  \w     35.00 102.00   0.50    1.00    --  107.75 -77.00 -90.00  134
 21  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00  30.00   66
 22  \w     94.00 174.00   0.50    1.00    --  107.75  15.00 -60.00  160
 23  \w     85.00 174.00   0.50    1.00    --  107.75  77.00-180.00  178
 24  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00 -90.00   66
 25  \w     35.00 102.00   0.50    1.00    --  107.75 -77.00-180.00  134
 26  \w     35.00  68.00   0.50    1.00    --  107.75 -61.00-120.00   66
 27  \w     33.00  88.00   0.50    0.25    --   47.95  57.00-120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0192695000
_diffrn_orient_matrix_UB_12      -0.0009936000
_diffrn_orient_matrix_UB_13      0.1622749000
_diffrn_orient_matrix_UB_21      0.1786267000
_diffrn_orient_matrix_UB_22      -0.0344771000
_diffrn_orient_matrix_UB_23      -0.0056879000
_diffrn_orient_matrix_UB_31      0.0824968000
_diffrn_orient_matrix_UB_32      0.0748816000
_diffrn_orient_matrix_UB_33      -0.0004400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15141
_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         77.189
_diffrn_reflns_theta_min         4.661
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.886
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0476P)^2^+1.0828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2927
_reflns_number_total             2995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02818e2.cif
_cod_data_source_block           19ma097_dv89
_cod_database_code               7706191
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.186
_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), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              15632
_olex2_submission_special_instructions 'No special instructions were received'