Cobalt(II) containing liquid metal salts for electrodeposition of cobalt and electrochemical nanoparticle formation
Sniekers, Jeroen; Geysens, Pieter; Malaquias, Joao; Vander Hoogerstraete, Tom; Van Meervelt, Luc; Fransaer, Jan; Binnemans, Koen; Dalton Trans.  (2017) –; doi:10.1039/C7DT02604H

data_7044160
_publ_section_title
;
 Cobalt(II) containing liquid metal salts for electrodeposition of cobalt
 and electrochemical nanoparticle formation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02604H
_journal_year                    2017
_chemical_formula_moiety         'C30 H48 Co N12, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C34 H48 Co F12 N14 O8 S4'
_chemical_formula_weight         1196.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-04-24 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.154(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0532(5)
_cell_length_b                   11.1257(5)
_cell_length_c                   20.1637(10)
_cell_measurement_reflns_used    6293
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7970
_cell_measurement_theta_min      3.4570
_cell_volume                     2454.6(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -88.00  -59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -38.0000    0.0000 29

  2 omega  -36.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   57.0000   90.0000 82

  3 omega  -23.00    9.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -38.0000 -150.0000 32

  4 omega    0.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000 -180.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0199216000
_diffrn_orient_matrix_UB_12      -0.0331473000
_diffrn_orient_matrix_UB_13      0.0295607000
_diffrn_orient_matrix_UB_21      -0.0016272000
_diffrn_orient_matrix_UB_22      0.0531050000
_diffrn_orient_matrix_UB_23      0.0193260000
_diffrn_orient_matrix_UB_31      -0.0617438000
_diffrn_orient_matrix_UB_32      -0.0121294000
_diffrn_orient_matrix_UB_33      0.0036364000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10709
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.742
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94058
_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    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0237P)^2^+1.7142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4447
_reflns_number_total             5012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02604h2.cif
_cod_data_source_block           kb2070
_cod_database_code               7044160
_chemical_oxdiff_formula         'Co C4 F12 S4 O8 N2 C24 H32 N12'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C15(H15A,H15B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C11(H11), C13(H13), C14(H14), C17(H17), C19(H19),
 C20(H20)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              99240
_shelx_shelxl_version_number     2016/4
_olex2_date_sample_data_collection 2014-10-08
_olex2_submission_special_instructions 'No special instructions were received'