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_7706192
_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           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-09
_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                 95.4270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.82730(10)
_cell_length_b                   13.99670(10)
_cell_length_c                   19.10800(10)
_cell_measurement_reflns_used    10246
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.8740
_cell_measurement_theta_min      3.9150
_cell_volume                     5545.27(6)
_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 2014/5 (Sheldrick, 2014)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.960
_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     33.00 120.00   0.50    3.05    --   47.95  77.00 -30.00  174
  2  \w     89.00 144.00   0.50   12.00    --  107.11 131.00   0.00  110
  3  \w     91.00 162.00   0.50   12.00    --  107.11  61.00  90.00  142
  4  \w    113.00 140.00   0.50   12.00    --  107.11  30.00   0.00   54
  5  \w    147.00 173.00   0.50   12.00    --  107.11  30.00 -60.00   52
  6  \w    136.00 173.00   0.50   12.00    --  107.11  45.00-180.00   74
  7  \w    102.00 130.00   0.50   12.00    --  107.11  30.00 -60.00   56
  8  \w     40.00  67.00   0.50   12.00    --  107.11 -61.00 -30.00   54
  9  \w     40.00  68.00   0.50   12.00    --  107.11 -61.00   0.00   56
 10  \w     69.00  95.00   0.50   12.00    --  107.11 -94.00 -60.00   52
 11  \w     35.00  99.00   0.50    3.05    --   47.95-131.00 -70.00  128
 12  \w     35.00 122.00   0.50   12.00    --  107.11-131.00 -70.00  174
 13  \w     39.00 103.00   0.50    3.05    --   47.95-138.00 114.00  128
 14  \w     66.00 124.00   0.50   12.00    --  107.11-138.00 114.00  116
 15  \w     38.00 102.00   0.50   12.00    --  107.11 -77.00  90.00  128
 16  \w     36.00  68.00   0.50   12.00    --  107.11 -61.00 -60.00   64
 17  \w     35.00  68.00   0.50   12.00    --  107.11 -61.00-120.00   66
 18  \w     35.00  68.00   0.50   12.00    --  107.11 -61.00 -90.00   66
 19  \w    -16.00  35.00   0.50    3.05    --   47.95 -38.00-120.00  102
 20  \w    -25.00  16.00   0.50    3.05    --   47.95 -19.00   0.00   82
 21  \w    -18.00  40.00   0.50    3.05    --   47.95 -38.00  30.00  116
 22  \w    -69.00 -13.00   0.50    3.05    --  -18.75 131.00   0.00  112
 23  \w    -73.00 -16.00   0.50    3.05    --  -18.75 138.00 175.00  114
 24  \w     84.00 174.00   0.50   12.00    --  107.11 138.00 175.00  180
;
_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      0.0381944000
_diffrn_orient_matrix_UB_12      0.0902948000
_diffrn_orient_matrix_UB_13      -0.0162535000
_diffrn_orient_matrix_UB_21      0.0561012000
_diffrn_orient_matrix_UB_22      -0.0628963000
_diffrn_orient_matrix_UB_23      -0.0201601000
_diffrn_orient_matrix_UB_31      -0.0302233000
_diffrn_orient_matrix_UB_32      -0.0026354000
_diffrn_orient_matrix_UB_33      -0.0767362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21839
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.175
_diffrn_reflns_theta_min         3.810
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       needle
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0515P)^2^+3.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5193
_reflns_number_total             5651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02818e2.cif
_cod_data_source_block           19MA093_DV91
_cod_database_code               7706192
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C184 H232 Cl16 Fe8 N40 O32 S16 '
_diffrn_oxdiff_digest_frames
;
018b58770624798f11a82cab6e467f61ef010096e0c
;
_diffrn_oxdiff_digest_hkl
;
014153857bffa786bf98f7a4739739da6ad0ba
;
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C34(H34), C32(H32), C35(H35), C14(H14), C27(H27), C28(H28), C16(H16),
 C31(H31), C15(H15), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C7(H7A,H7B,H7C), C11(H11A,H11B,
 H11C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              73929
_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 3.013
_oxdiff_exptl_absorpt_empirical_full_min 0.455