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_7044165
_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
'C21 H36 Co0.5 N6, C21 H35 Co0.5 N6, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C46 H71 Co F12 N14 O8 S4'
_chemical_formula_weight         1363.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-04
_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                88.258(3)
_cell_angle_beta                 89.339(3)
_cell_angle_gamma                80.363(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6957(3)
_cell_length_b                   17.4965(6)
_cell_length_c                   18.8465(6)
_cell_measurement_reflns_used    10390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9100
_cell_measurement_theta_min      3.2500
_cell_volume                     3150.49(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -88.00   18.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -19.0000  -90.0000 106

  2 omega  -87.00    6.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -77.0000   90.0000 93

  3 omega  -40.00   -2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -57.0000  -30.0000 38

  4 omega  -85.00    4.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -57.0000 -150.0000 89

  5 omega  -23.00    6.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -65.0000  109.0000 29

  6 omega   10.00   50.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   77.0000  -60.0000 40
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0099899000
_diffrn_orient_matrix_UB_12      -0.0244584000
_diffrn_orient_matrix_UB_13      -0.0281630000
_diffrn_orient_matrix_UB_21      -0.0729837000
_diffrn_orient_matrix_UB_22      0.0140100000
_diffrn_orient_matrix_UB_23      0.0010459000
_diffrn_orient_matrix_UB_31      0.0089418000
_diffrn_orient_matrix_UB_32      0.0299627000
_diffrn_orient_matrix_UB_33      -0.0249714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24409
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90917
_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    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         12848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0301P)^2^+2.5727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11114
_reflns_number_total             12848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02604h2.cif
_cod_data_source_block           kb2078
_cod_original_cell_volume        3150.49(19)
_cod_database_code               7044165
_chemical_oxdiff_formula         'Co C4 F12 S4 O8 N2 N12 C40 H60'
_reflns_odcompleteness_completeness 99.85
_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:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C35(H35), C36(H36), C41(H41), C43(H43), C44(H44), C49(H49),
 C51(H51), C52(H52), C11(H11), C12(H12), C17(H17), C19(H19), C20(H20), C25(H25),
  C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              42611
_shelx_shelxl_version_number     2016/4
_olex2_date_sample_data_collection 2014-11-04
_olex2_submission_special_instructions 'No special instructions were received'