Synthesis and characterization of a series of acylpyrazolone transition metal complexes: Crystal structures and catalytic performance in the epoxidation of cyclooctene
Hasanzadeh Esfahani, Maryam; Behzad, Mahdi; Dusek, Michal; Kucerakova, Monika; Inorganica Chimica Acta 508 (2020) 119637–; doi:10.1016/j.ica.2020.119637

data_1564582
_publ_section_title
;
 Synthesis and characterization of a series of acylpyrazolone transition
 metal complexes: Crystal structures and catalytic performance in the
 epoxidation of cyclooctene
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119637
_journal_paper_doi               10.1016/j.ica.2020.119637
_journal_volume                  508
_journal_year                    2020
_chemical_absolute_configuration .
_chemical_formula_moiety         'C36 H33 Fe N6 O6'
_chemical_formula_sum            'C36 H33 Fe N6 O6'
_chemical_formula_weight         701.5
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                71.394(3)
_cell_angle_beta                 85.959(3)
_cell_angle_gamma                83.585(3)
_cell_formula_units_Z            4
_cell_length_a                   9.2630(3)
_cell_length_b                   18.2874(6)
_cell_length_c                   20.6851(7)
_cell_measurement_reflns_used    4817
_cell_measurement_temperature    95.00(10)
_cell_measurement_theta_max      73.89
_cell_measurement_theta_min      4.49
_cell_volume                     3297.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_diffrn_ambient_temperature      95
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2027
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20221
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program CrysAlisPro
(Agilent Technologies, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        69.91
_diffrn_reflns_theta_max         74.47
_diffrn_reflns_theta_min         3.91
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.139
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       'polygon shape'
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.30
_refine_ls_goodness_of_fit_ref   1.22
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    264
_refine_ls_number_parameters     883
_refine_ls_number_reflns         12817
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.0162
_refine_ls_shift/su_mean         0.0021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                8680
_reflns_number_total             12817
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ICA-2020-508-119637.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 

2022-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1403.1
_cod_original_formula_moiety         'Fe2 N12 O12 C72 H66'
_cod_original_formula_units_Z            2
_cod_original_formula_sum        'Fe2 N12 O12 C72 H66'
_cod_database_code               1564582