Manganese-containing ionic liquids: synthesis, crystal structures and electrodeposition of manganese films and nanoparticles.
Sniekers, Jeroen; Malaquias, João C; Van Meervelt, Luc; Fransaer, Jan; Binnemans, Koen; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2497–2509; doi:10.1039/c6dt04781e

data_7041824
_publ_section_title
;
 Manganese-containing ionic liquids: synthesis, crystal structures and
 electrodeposition of manganese films and nanoparticles.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2497
_journal_page_last               2509
_journal_paper_doi               10.1039/c6dt04781e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C12 H18 F12 Mn N2 O12 S4'
_chemical_formula_sum            'C12 H18 F12 Mn N2 O12 S4'
_chemical_formula_weight         793.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-26 deposited with the CCDC.
2017-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.801(2)
_cell_length_b                   15.0805(11)
_cell_length_c                   8.9654(5)
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.7840
_cell_measurement_theta_min      3.6740
_cell_volume                     5381.2(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
  1 omega  -35.00   -6.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.3117   57.0000  -30.0000 29

  2 omega  -58.00   58.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.3117   19.0000   90.0000 116
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0025034000
_diffrn_orient_matrix_UB_12      -0.0455559000
_diffrn_orient_matrix_UB_13      -0.0163422000
_diffrn_orient_matrix_UB_21      -0.0174663000
_diffrn_orient_matrix_UB_22      0.0050015000
_diffrn_orient_matrix_UB_23      0.0132809000
_diffrn_orient_matrix_UB_31      -0.0024969000
_diffrn_orient_matrix_UB_32      0.0106013000
_diffrn_orient_matrix_UB_33      -0.0762552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3703
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.889
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.086(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2202
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+328.2570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1802
_reflns_Friedel_coverage         0.568
_reflns_Friedel_fraction_full    0.678
_reflns_Friedel_fraction_max     0.622
_reflns_number_gt                2187
_reflns_number_total             2202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04781e2.cif
_cod_data_source_block           kb2026
_cod_depositor_comments
'Adding full bibliography for 7041822--7041828.cif.'
_cod_original_cell_volume        5381.2(5)
_cod_database_code               7041824
_chemical_oxdiff_formula         'Mn C4 F12 S4 O8 N2 C8 H16 O4 H4 O2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O4) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(S16)
\\sim Ueq, Uanis(S13) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2013-11-15
_olex2_submission_special_instructions 'No special instructions were received'