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_7706193
_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         'I, C27 H26 Cl Fe N6 O'
_chemical_formula_sum            'C27 H26 Cl Fe I N6 O'
_chemical_formula_weight         668.74
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-26
_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                 97.2461(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.64797(16)
_cell_length_b                   15.77189(15)
_cell_length_c                   9.27194(8)
_cell_measurement_reflns_used    13267
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      27.3910
_cell_measurement_theta_min      1.6470
_cell_volume                     2850.29(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      173.01(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   18.00    --   27.42  77.00-180.00  128
  2  \w     35.00 122.00   1.00   18.00    --   27.42 178.00  90.00   87
  3  \w     35.00 122.00   1.00   18.00    --   27.42 178.00 -90.00   87
  4  \w    -49.00  65.00   1.00   18.00    --   27.42 -57.00  90.00  114
  5  \w    -10.00 103.00   1.00   18.00    --   27.42  57.00 -30.00  113
  6  \w    -54.00  27.00   1.00   18.00    --   27.42 -38.00-150.00   81
  7  \w    -10.00 103.00   1.00   18.00    --   27.42  57.00  60.00  113
;
_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      -0.0321229000
_diffrn_orient_matrix_UB_12      -0.0201671000
_diffrn_orient_matrix_UB_13      -0.0193532000
_diffrn_orient_matrix_UB_21      -0.0165639000
_diffrn_orient_matrix_UB_22      0.0400286000
_diffrn_orient_matrix_UB_23      -0.0031275000
_diffrn_orient_matrix_UB_31      0.0042677000
_diffrn_orient_matrix_UB_32      0.0035681000
_diffrn_orient_matrix_UB_33      -0.0745970000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30955
_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         28.156
_diffrn_reflns_theta_min         1.661
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.550
_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    1.558
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0345P)^2^+1.6337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5462
_reflns_number_total             6497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02818e2.cif
_cod_data_source_block           19ma034c_dv66
_cod_database_code               7706193
_shelx_shelxl_version_number     2018/1
_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), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              39998
_olex2_submission_special_instructions 'No special instructions were received'