Structure and catalytic properties of novel copper isatin Schiff base complexes
Smirnov, Andrey S.; Martins, Luísa M. D. R. S.; Nikolaev, Dmitriy N.; Manzhos, Roman A.; Gurzhiy, Vlad V.; Krivenko, Alexander G.; Nikolaenko, Kirill O.; Belyakov, Alexander V.; Garabadzhiu, Alexander V.; Davidovich, Pavel B.; New Journal of Chemistry 43 (2019) 188–; doi:10.1039/C8NJ02718H

data_7057892
_publ_section_title
;
 Structure and catalytic properties of novel copper isatin Schiff base
 complexes
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              188
_journal_paper_doi               10.1039/C8NJ02718H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C38 H39 Cu N5 O2, B F4, 0.3(H2O)'
_chemical_formula_sum            'C38 H39 B Cu F4 N5 O2.3'
_chemical_formula_weight         752.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-19 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.297(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8485(3)
_cell_length_b                   14.2133(3)
_cell_length_c                   21.2613(5)
_cell_measurement_reflns_used    10018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9470
_cell_measurement_theta_min      3.4670
_cell_volume                     3726.72(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -35.00   -8.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.9969  -19.0000   30.0000 27

  2 omega  -48.00   16.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.9969  -57.0000  120.0000 64

  3 omega    4.00   44.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       12.8719  -99.0000  120.0000 40

  4 omega  -57.00   17.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       12.8719  -38.0000 -120.0000 74

  5 omega  -30.00    2.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.9969   38.0000 -150.0000 32

  6 omega    7.00   32.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.9969   38.0000 -150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0156390000
_diffrn_orient_matrix_UB_12      -0.0467443000
_diffrn_orient_matrix_UB_13      -0.0100312000
_diffrn_orient_matrix_UB_21      -0.0119315000
_diffrn_orient_matrix_UB_22      0.0140255000
_diffrn_orient_matrix_UB_23      -0.0332886000
_diffrn_orient_matrix_UB_31      0.0540361000
_diffrn_orient_matrix_UB_32      -0.0104079000
_diffrn_orient_matrix_UB_33      0.0001330000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25734
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       prism
_exptl_crystal_F_000             1562
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.148
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8807
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0547P)^2^+5.3371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7026
_reflns_number_total             8807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02718h2.cif
_cod_data_source_block           as115
_cod_depositor_comments
'Adding full bibliography for 7057891--7057914.cif.'
_cod_original_formula_sum        'C38 H39 B Cu F4 N5 O2.30'
_cod_database_code               7057892
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Restrained distances
 O31A-O31B
 1.2 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(F28A) = Uanis(F28B) = Uanis(F29A) = Uanis(F29B) = Uanis(F30A) =
Uanis(F30B)
Uanis(O31A) = Uanis(O31B)
4. Others
 Sof(F28B)=Sof(F29B)=Sof(F30B)=1-FVAR(1)
 Sof(F28A)=Sof(F29A)=Sof(F30A)=FVAR(1)
 Fixed Sof: O31A(0.21) O31B(0.09)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C6'(H6'), C7(H7), C7'(H7'), C8(H8), C8'(H8'), C9(H9), C9'(H9'),
 C15(H15), C15'(H15'), C17(H17), C17'(H17')
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C10'(H10D,H10E,H10F), C19(H19A,H19B,H19C), C19'(H19D,
 H19E,H19F), C20(H20A,H20B,H20C), C20'(H20D,H20E,H20F), C21(H21A,H21B,H21C),
 C21'(H21D,H21E,H21F), C25(H25A,H25B,H25C)
;