Photochromism and hydrochromism of three complexes based on a new viologen 1-(4-carboxybutyl)-4,4′-bipyridinium ligand
Li, Jing; Liu, Jinjian; Lu, Wenbo; Inorganica Chimica Acta 512 (2020) 119921–; doi:10.1016/j.ica.2020.119921

data_1564122
_publ_section_title
;
 Photochromism and hydrochromism of three complexes based on a new
 viologen 1-(4-carboxybutyl)-4,4&#x2032;-bipyridinium ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119921
_journal_paper_doi               10.1016/j.ica.2020.119921
_journal_volume                  512
_journal_year                    2020
_chemical_formula_moiety         'C20 H25 N2 O10 Zn, 3(H2 O), C5 H O4'
_chemical_formula_sum            'C25 H32 N2 O17 Zn'
_chemical_formula_weight         697.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                84.655(5)
_cell_angle_beta                 87.829(4)
_cell_angle_gamma                71.917(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3553(4)
_cell_length_b                   10.2916(6)
_cell_length_c                   18.6070(12)
_cell_measurement_reflns_used    3772
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      72.2610
_cell_measurement_theta_min      6.6440
_cell_volume                     1514.30(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      273(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -77.00 -34.00   1.00    1.00    --    0.00 178.00 120.00   43
  2  \w    -19.00  18.00   1.00    1.00    --    0.00  57.00  30.00   37
  3  \w    -62.00 -35.00   1.00    1.00    --    0.00 178.00 -60.00   27
  4  \w     36.00  61.00   1.00    1.00    --    0.00  57.00  30.00   25
  5  \w     34.00  69.00   1.00    1.00    --   55.26 -57.00-180.00   35
  6  \w     31.00 108.00   1.00    1.00    --   55.26  38.00  30.00   77
  7  \w     -4.00  81.00   1.00    1.00    --   55.26 -38.00-150.00   85
  8  \w     36.00  90.00   1.00    1.00    --   55.26  57.00  90.00   54
  9  \w    -10.00  76.00   1.00    1.00    --   55.26 -38.00 120.00   86
 10  \w     39.00  75.00   1.00    1.00    --   55.26 -99.00   0.00   36
 11  \w     40.00 110.00   1.00    1.00    --   55.26-125.00-180.00   70
 12  \w     51.00  98.00   1.00    1.00    --   55.26 -19.00   0.00   47
 13  \w    -11.00  14.00   1.00    1.00    --   55.26 -19.00   0.00   25
 14  \w     38.00 177.00   1.00    1.00    --  110.51   0.00-150.00  139
 15  \w     38.00  96.00   1.00    1.00    --  110.51-111.00 -60.00   58
 16  \w    116.00 170.00   1.00    1.00    --  110.51 111.00   0.00   54
 17  \w    109.00 155.00   1.00    1.00    --  110.51  50.00-120.00   46
 18  \w     67.00 115.00   1.00    1.00    --  110.51-111.00-150.00   48
 19  \w     48.00 108.00   1.00    1.00    --  110.51-111.00  30.00   60
 20  \w    138.00 171.00   1.00    1.00    --  110.51  77.00 150.00   33
 21  \w     41.00 126.00   1.00    1.00    --  110.51 -50.00  90.00   85
 22  \w    109.00 136.00   1.00    1.00    --  110.51 -38.00-150.00   27
 23  \w     72.00  98.00   1.00    1.00    --  110.51 -38.00-150.00   26
 24  \w     69.00  95.00   1.00    1.00    --  110.51-111.00  90.00   26
 25  \w     43.00 128.00   1.00    1.00    --  110.51 -50.00   0.00   85
 26  \w    123.00 171.00   1.00    1.00    --  110.51 111.00  90.00   48
 27  \w     97.00 162.00   1.00    1.00    --  110.51  64.00  60.00   65
 28  \w     85.00 110.00   1.00    1.00    --  110.51  77.00 150.00   25
 29  \w     64.00  97.00   1.00    1.00    --  110.51-111.00 150.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0288930000
_diffrn_orient_matrix_UB_12      0.0171858000
_diffrn_orient_matrix_UB_13      0.0793797000
_diffrn_orient_matrix_UB_21      -0.0279031000
_diffrn_orient_matrix_UB_22      -0.1391729000
_diffrn_orient_matrix_UB_23      0.0228842000
_diffrn_orient_matrix_UB_31      0.1897646000
_diffrn_orient_matrix_UB_32      -0.0729066000
_diffrn_orient_matrix_UB_33      -0.0095263000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.316
_diffrn_reflns_theta_min         4.536
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         5837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0706P)^2^+0.7522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4967
_reflns_number_total             5837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119921.cif
_cod_data_source_block           Zn
_cod_database_code               1564122
_chemical_oxdiff_formula         'C H O N Br Zn'
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.708
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H,H) groups
2.a Free rotating group:
 O17(H17A,H17B), O16(H16A,H16B), O15(H15A,H15B)
2.b Rotating group:
 O5(H5A,H5B), O3(H3A,H3B), O6(H6A,H6B), O4(H4C,H4D)
2.c Secondary CH2 refined with riding coordinates:
 C5(H5C,H5D), C4(H4A,H4B), C3(H3C,H3D), C2(H2A,H2B)
2.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C14(H14), C15(H15), C9(H9), C24(H24), C12(H12), C8(H8), C7(H7),
 C13(H13), C6(H6)
;
_shelx_res_checksum              34616
_shelx_hkl_checksum              25313