Dissolution of metal oxides in task-specific ionic liquid
Richter, Janine; Ruck, Michael; RSC Advances 9 (2019) 29699–; doi:10.1039/C9RA06423K

data_7233992
_publ_section_title
;
 Dissolution of metal oxides in task-specific ionic liquid
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              29699
_journal_paper_doi               10.1039/C9RA06423K
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C24 H44 Cu2 F12 N6 O16 S4, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C28 H44 Cu2 F24 N8 O24 S8'
_chemical_formula_weight         1716.27
_chemical_name_systematic
'Tetrakis(betaine)bis(bis(trifluoromethane)sulfonimide)dicuprate(II) bis(trifluoromethane)sulfonimide'
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-16 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.182(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4550(4)
_cell_length_b                   14.4844(6)
_cell_length_c                   14.9892(4)
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4440
_cell_measurement_theta_min      4.0540
_cell_volume                     3125.49(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.15e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.15e (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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   -106.00 -66.00   1.00   21.16    --  -41.18 -57.00   0.00   40
  2  \w    -68.00  32.00   1.00   21.16    --  -41.18  57.00 150.00  100
  3  \w    -43.00 -16.00   1.00   21.16    --  -41.18 -57.00   0.00   27
  4  \w     88.00 115.00   1.00   21.16    --   41.18  38.00  30.00   27
  5  \w     17.00  65.00   1.00   21.16    --   41.18 -99.00-150.00   48
  6  \w    148.00 173.00   1.00   52.83    --  112.00 111.00  60.00   25
  7  \w     36.00 107.00   1.00   52.83    --  112.00-111.00  60.00   71
  8  \w     71.00 110.00   1.00   52.83    --  112.00 -61.00  60.00   39
  9  \w     65.00  92.00   1.00   52.83    --  112.00 -61.00 120.00   27
 10  \w     76.00 113.00   1.00   52.83    --  112.00-111.00  90.00   37
 11  \w    110.00 141.00   1.00   52.83    --  112.00 -61.00 120.00   31
 12  \w    100.00 147.00   1.00   52.83    --  112.00 111.00 177.00   47
 13  \w    148.00 174.00   1.00   52.83    --  112.00  77.00  90.00   26
 14  \w     38.00  70.00   1.00   52.83    --  112.00-111.00 150.00   32
 15  \w     44.00  70.00   1.00   52.83    --  112.00 -94.00 -30.00   26
 16  \w     37.00  73.00   1.00   52.83    --  112.00-111.00  90.00   36
 17  \w    132.00 162.00   1.00   52.83    --  112.00  45.00-180.00   30
 18  \w     81.00 106.00   1.00   52.83    --  112.00 -94.00 120.00   25
 19  \w     94.00 143.00   1.00   52.83    --  112.00  45.00   0.00   49
 20  \w     77.00 110.00   1.00   52.83    --  112.00 -77.00  60.00   33
 21  \w     71.00 137.00   1.00   52.83    --  112.00 -45.00  60.00   66
 22  \w     43.00  68.00   1.00   52.83    --  112.00 -30.00-180.00   25
 23  \w     87.00 177.00   1.00   52.83    --  112.00  45.00 120.00   90
 24  \w     44.00 113.00   1.00   52.83    --  112.00-111.00-120.00   69
 25  \w     37.00  62.00   1.00   52.83    --  112.00 -30.00-120.00   25
 26  \w     84.00 109.00   1.00   52.83    --  112.00  77.00  90.00   25
 27  \w     87.00 112.00   1.00   52.83    --  112.00-111.00 150.00   25
 28  \w     35.00  62.00   1.00   52.83    --  112.00 -15.00  30.00   27
 29  \w    122.00 147.00   1.00   52.83    --  112.00 -15.00  30.00   25
 30  \w    120.00 145.00   1.00   52.83    --  112.00  77.00 120.00   25
 31  \w     84.00 174.00   1.00   52.83    --  112.00  30.00-150.00   90
 32  \w    144.00 170.00   1.00   52.83    --  112.00  61.00  60.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0677164000
_diffrn_orient_matrix_UB_12      0.0673927000
_diffrn_orient_matrix_UB_13      0.0518456000
_diffrn_orient_matrix_UB_21      0.0693947000
_diffrn_orient_matrix_UB_22      -0.0794452000
_diffrn_orient_matrix_UB_23      0.0203901000
_diffrn_orient_matrix_UB_31      0.0451869000
_diffrn_orient_matrix_UB_32      0.0217834000
_diffrn_orient_matrix_UB_33      -0.0868411000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24246
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.029
_diffrn_reflns_theta_min         4.069
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.15e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_recrystallization_method
'Crystal obtained from the IL without any recrystalisation or washing.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0603P)^2^+2.4034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5133
_reflns_number_total             6538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra06423k2.cif
_cod_data_source_block           jr-cuo
_cod_database_code               7233992
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.452
_shelx_estimated_absorpt_t_min   0.452
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              32724
_ins_header
;
TITL JR-CuO in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  14.454994  14.484391  14.989207  90.0000  95.1819  90.0000
ZERR   14.00   0.000450   0.000556   0.000450   0.0000   0.0029   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O
UNIT 154.00 140.00 14.00 14.00
TREF
HKLF 4
END
;
_olex2_date_sample_data_collection 2018-10-21
_olex2_submission_original_sample_id '[Cu2(bet)4(NTf2)2][NTf2]2'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.516
_oxdiff_exptl_absorpt_empirical_full_min 0.469