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_1564579
_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         'C30 H36 Mn1 N6 O6'
_chemical_formula_sum            'C30 H36 Mn N6 O6'
_chemical_formula_weight         631.6
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.028(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7828(3)
_cell_length_b                   17.1305(6)
_cell_length_c                   9.9907(3)
_cell_measurement_reflns_used    6938
_cell_measurement_temperature    119.96(13)
_cell_measurement_theta_max      67.51
_cell_measurement_theta_min      5.16
_cell_volume                     1470.14(9)
_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      119.96
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1783
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_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  0.0226
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11536
_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        67.61
_diffrn_reflns_theta_max         67.61
_diffrn_reflns_theta_min         5.16
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.106
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.738
_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            white
_exptl_crystal_density_diffrn    1.4268
_exptl_crystal_description       'polygon shape'
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.44
_refine_ls_goodness_of_fit_ref   1.42
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    72
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.0084
_refine_ls_shift/su_mean         0.0013
_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          0.0721
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                2462
_reflns_number_total             2633
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ICA-2020-508-119637.cif
_cod_data_source_block           I
_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 
;
_cod_original_sg_symbol_Hall     '-P 2yabc'
_cod_original_formula_sum        'Mn N6 O6 C30 H36'
_cod_database_code               1564579