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_7057900
_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         'C30 H24 Br Cu N4 O4'
_chemical_formula_sum            'C30 H24 Br Cu N4 O4'
_chemical_formula_weight         647.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2017-03-19 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.316(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9161(9)
_cell_length_b                   6.9866(5)
_cell_length_c                   21.0116(9)
_cell_measurement_reflns_used    1484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2970
_cell_measurement_theta_min      4.1960
_cell_volume                     2629.4(3)
_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    'ShelXT (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 0.9864
_diffrn_measured_fraction_theta_max 0.9585
_diffrn_measurement_details
;
  1 omega -103.00  -66.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787 -150.0000  168.0000 37

  2 omega  -46.00  -17.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -32.0000   33.0000 29

  3 omega -114.00  -16.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000  150.0000 98

  4 omega   59.00  128.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000   90.0000 69

  5 omega   95.00  121.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000 -180.0000 26

  6 omega   50.00  107.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 57

  7 omega   35.00   71.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 36

  8 omega   39.00   78.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 39

  9 omega   82.00  115.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 33

 10 omega   35.00   85.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 50

 11 omega  142.00  177.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 35

 12 omega   72.00  113.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   60.0000 41

 13 omega  136.00  178.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -150.0000 42

 14 omega   42.00   97.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 55

 15 omega   58.00  125.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -30.0000 67
;
_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      -0.0093166000
_diffrn_orient_matrix_UB_12      -0.2163150000
_diffrn_orient_matrix_UB_13      0.0112700000
_diffrn_orient_matrix_UB_21      0.0772515000
_diffrn_orient_matrix_UB_22      -0.0361800000
_diffrn_orient_matrix_UB_23      -0.0285499000
_diffrn_orient_matrix_UB_31      0.0369190000
_diffrn_orient_matrix_UB_32      0.0212337000
_diffrn_orient_matrix_UB_33      0.0665571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4917
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.490
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26707
_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            orange
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1958
_refine_ls_wR_factor_ref         0.2125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2011
_reflns_number_total             2547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02718h2.cif
_cod_data_source_block           pd_157
_cod_depositor_comments
'Adding full bibliography for 7057891--7057914.cif.'
_cod_database_code               7057900
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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, All O(H) groups
2. Restrained distances
 O19A-H19A = O19B-H19B
 0.9 with sigma of 0.02
 Br21_$1-H19B
 2.5 with sigma of 0.02
 O19B-C14
 1.3 with sigma of 0.02
3. Others
 Sof(H18)=Sof(O19B)=Sof(H19B)=1-FVAR(1)
 Sof(H14)=Sof(O19A)=Sof(H19A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;