Water-stable [Ni(salen)]-type electrode material based on phenylazosubstituted salicylic aldehyde imine ligand
Vereshchagin, Anatoliy A.; Sizov, Vladimir; Vlasov, Petr; Alekseeva, Elena V.; Konev, Alexander S.; Levin, Oleg V.; New J. Chem. 41 (2017) 13918–13928; doi:10.1039/C7NJ03526H

data_7056680
_publ_section_title
;
 Water-stable [Ni(salen)]-type electrode material based on
 phenylazosubstituted salicylic aldehyde imine ligand
;
_journal_issue                   22
_journal_name_full               'New J. Chem.'
_journal_page_first              13918
_journal_page_last               13928
_journal_paper_doi               10.1039/C7NJ03526H
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C28 H22 N6 Ni O2, C2 H6 O S, 0.8(H2 O1)'
_chemical_formula_sum            'C30 H29 N6 Ni O3.75 S'
_chemical_formula_weight         624.36
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-04-12 deposited with the CCDC.
2017-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.105(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5639(5)
_cell_length_b                   29.9290(12)
_cell_length_c                   10.7888(5)
_cell_measurement_reflns_used    4934
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.7620
_cell_measurement_theta_min      4.7890
_cell_volume                     2773.1(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -43.00   28.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4354   38.0000   90.0000 71

  2 omega -109.00  -17.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4354  -38.0000  -90.0000 92

  3 omega   91.00  123.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4354  178.0000  150.0000 32

  4 omega   74.00  121.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4354  178.0000    0.0000 47

  5 omega   88.00  117.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 29

  6 omega   53.00   91.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 38

  7 omega   40.00   66.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -120.0000 26

  8 omega   62.00   91.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 29

  9 omega   38.00   69.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 31

 10 omega   42.00   90.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 48

 11 omega   76.00  119.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000    0.0000 43

 12 omega  132.00  175.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  120.0000 43

 13 omega   50.00   93.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -30.0000 43

 14 omega   99.00  162.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000    0.0000 63

 15 omega   69.00   96.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000    0.0000 27

 16 omega   46.00   90.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  150.0000 44

 17 omega   41.00   76.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000    0.0000 35

 18 omega   55.00   96.00   1.0000  186.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -90.0000 41
;
_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      -0.0629751000
_diffrn_orient_matrix_UB_12      0.0274968000
_diffrn_orient_matrix_UB_13      0.0853278000
_diffrn_orient_matrix_UB_21      -0.1023028000
_diffrn_orient_matrix_UB_22      0.0272859000
_diffrn_orient_matrix_UB_23      -0.1294780000
_diffrn_orient_matrix_UB_31      -0.1332656000
_diffrn_orient_matrix_UB_32      -0.0338923000
_diffrn_orient_matrix_UB_33      -0.0351631000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65438
_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_colour_primary    red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       needle
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.495
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5235
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0928P)^2^+1.1003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4459
_reflns_number_total             5235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03526h2.cif
_cod_data_source_block           103-245-2794_1
_cod_original_cell_volume        2773.2(3)
_cod_database_code               7056680
_chemical_oxdiff_formula         'C28 N6 O2 Ni H14'
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1B
 1 with sigma of 0.05
 O1-H1B
 1 with sigma of 0.05
3. Others
 Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(S6)=1-FVAR(1)
 Sof(S1)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(2)
4.a Free rotating group:
 O1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 C95(H95A,H95B), C102(H10A,H10B)
4.c Me refined with riding coordinates:
 C71(H71A,H71B,H71C), C71(H71D,H71E,H71F), C125(H12A,H12B,H12C), C125(H12D,
 H12E,H12F)
4.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C18(H18), C33(H33), C47(H47), C57(H57), C68(H68), C73(H73), C76(H76),
 C85(H85), C90(H90), C92(H92), C93(H93), C98(H98), C100(H100), C108(H108),
 C115(H115), C117(H117), C121(H121)
;
_shelx_res_checksum              79244
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'