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_1564121
_publ_section_title
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 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         'C15 H27 N2 Ni O7, C9 H3 O6, 5.5(H2 O)'
_chemical_formula_sum            'C24 H41 N2 Ni O18.5'
_chemical_formula_weight         712.30
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 117.905(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.1546(15)
_cell_length_b                   13.9895(9)
_cell_length_c                   22.906(2)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.28
_cell_volume                     6273.8(8)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44439
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.1271 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.8541.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.875
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1185P)^2^+19.7148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.1941
_reflns_number_gt                6863
_reflns_number_total             7807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-512-119921.cif
_cod_data_source_block           Ni
_cod_original_cell_volume        6273.7(8)
_cod_original_formula_sum        'C24 H41 N2 Ni O18.50'
_cod_database_code               1564121
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H3A,H3B} of C3, H18 of C18, {H2A,H2B} of C2, {H4A,H4B} of C4, H13 of C13,
  H9 of C9, H14 of C14, H12 of C12, H7 of C7, H8 of C8, H6 of C6, {H5A,H5B} of
  C5, H24 of C24, H21 of C21, H15 of C15
 At 1.5 times of:
  {H4C,H4D} of O4, {H18A,H18B} of O18, {H6A,H6B} of O6, {H16A,H16B} of O16,
  {H14A,H14B} of O14, {H19A,H19B} of O19, {H5C,H5D} of O5, {H1A,H1B} of O1, H2
  of O2, {H17A,H17B} of O17, {H15A,H15B} of O15, {H13A,H13B} of O13
2. Others
 Fixed Sof: H19A(0.5) H19B(0.5)
3.a Free rotating group:
 O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B), O6(H6A,H6B), O1(H1A,H1B),
 O5(H5C,H5D), O19(H19A,H19B), O4(H4C,H4D), O18(H18A,H18B)
3.b Rotating group:
 O14(H14A,H14B), O16(H16A,H16B)
3.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
3.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C9(H9), C14(H14), C12(H12), C7(H7), C8(H8), C6(H6),
 C24(H24), C21(H21), C18(H18)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
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