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_7044162
_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         'C42 H72 Co1 N12, 2(C1 H3 O3 S1)'
_chemical_formula_sum            'C44 H78 Co N12 O6 S2'
_chemical_formula_weight         994.23
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-07 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.4995(7)
_cell_length_b                   13.4995(7)
_cell_length_c                   25.8633(14)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8110
_cell_measurement_theta_min      3.5560
_cell_volume                     4081.8(4)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -45.00   47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   77.0000 -180.0000 92

  2 omega   57.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   77.0000   90.0000 26

  3 omega   -6.00   21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   77.0000 -180.0000 27

  4 omega   -8.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   77.0000   60.0000 95
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0383097000
_diffrn_orient_matrix_UB_12      0.0200751000
_diffrn_orient_matrix_UB_13      0.0057796000
_diffrn_orient_matrix_UB_21      0.0470424000
_diffrn_orient_matrix_UB_22      0.0560143000
_diffrn_orient_matrix_UB_23      0.0036094000
_diffrn_orient_matrix_UB_31      -0.0019090000
_diffrn_orient_matrix_UB_32      0.0118978000
_diffrn_orient_matrix_UB_33      -0.0265578000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            6466
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61482
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             1599
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0574P)^2^+15.8680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1736
_reflns_number_total             1863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02604h2.cif
_cod_data_source_block           kb2101
_cod_original_cell_volume        4081.8(5)
_cod_database_code               7044162
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Co C2 S2 O6 N12 C50 H80'
_reflns_odcompleteness_completeness 99.84
_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. Others
 Fixed Sof: H13A(0.33333) H13B(0.33333) H13C(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              62317
_olex2_submission_special_instructions 'No special instructions were received'