Mixed chloridometallate(ii) ionic liquids with tunable color and optical response for potential ammonia sensors
Behrens, Karsten; Balischewski, Christian; Sperlich, Eric; Menski, Antonia; Balderas-Valadez, Ruth Fabiola; Pacholski, Claudia; Günter, Christina; Lubahn, Susanne; Kelling, Alexandra; Taubert, Andreas; RSC Advances 12 (2022) 35072–35082; doi:10.1039/D2RA05581C

data_7245985
_publ_section_title
;
 Mixed chloridometallate(ii) ionic liquids with tunable color and optical
 response for potential ammonia sensors
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              35072
_journal_page_last               35082
_journal_paper_doi               10.1039/D2RA05581C
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         '4(C9 H14 N), 2(Cl4 Co0.50 Ni0.50)'
_chemical_formula_sum            'C36 H56 Cl8 Co N4 Ni'
_chemical_formula_weight         946.08
_chemical_name_systematic
; 
 Bis(N-butylpyridinium) tetrachlorido-0.5-cobaltate(II)-0.5-nickelate(II)
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-11 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.494(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3911(4)
_cell_length_b                   18.7389(5)
_cell_length_c                   16.7383(4)
_cell_measurement_reflns_used    92173
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.60
_cell_volume                     4522.0(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.86, Darmstadt 2018
SHELXL-2018/3 (Sheldrick, 2018)
Diamond (Blankenburg, 2020)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
; 
 5466 frames, exposure time = 5 s per frame,
 detector distance = 60 mm, \D\w = 0.5 \%
;
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.3 mm diameter'
_diffrn_radiation_monochromator  'graded multilayer mirror'
_diffrn_radiation_source         'Genix Microfocus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            157301
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.480
_diffrn_source_current           1.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.6748
_exptl_absorpt_correction_T_min  0.2210
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_exptl_crystal_size_rad          0.181
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0332P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5898
_reflns_number_total             7941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05581c2.cif
_cod_data_source_block           Behr10p
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7245985
_shelx_res_checksum              94187