Cobalt(ii) liquid metal salts for high current density electrodeposition of cobalt.
Sniekers, Jeroen; Geysens, Pieter; Vander Hoogerstraete, Tom; Van Meervelt, Luc; Fransaer, Jan; Binnemans, Koen; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4975–4986; doi:10.1039/C8DT00283E

data_7045760
_publ_section_title
;
 Cobalt(ii) liquid metal salts for high current density electrodeposition
 of cobalt.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4975
_journal_page_last               4986
_journal_paper_doi               10.1039/C8DT00283E
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C36 H24 Co N6, 2(C2 F6 N O4 S2), 0.5(C7 H8), 0.25(C7 H7)'
_chemical_formula_sum            'C45.25 H29.75 Co F12 N8 O8 S4'
_chemical_formula_weight         1228.69
_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             2017-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-25 deposited with the CCDC.
2018-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9636(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3290(2)
_cell_length_b                   23.1050(3)
_cell_length_c                   23.1472(3)
_cell_measurement_reflns_used    17256
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      28.9520
_cell_measurement_theta_min      2.7930
_cell_volume                     9765.9(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      99.97(11)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -10.00 23.00 1.0000 150.0000 omega____ theta____ kappa____ phi______ frames - -17.0732 -99.0000 0.0000 33 #__ type_ start__ end____ width___ exp.time_ 2 omega -57.00 49.00 1.0000 150.0000 omega____ theta____ kappa____ phi______ frames - -17.0732 19.0000 90.0000 106 #__ type_ start__ end____ width___ exp.time_ 3 omega -86.00 -2.00 1.0000 150.0000 omega____ theta____ kappa____ phi______ frames - -17.0732 -57.0000 90.0000 84'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0376143000
_diffrn_orient_matrix_UB_12      -0.0076472000
_diffrn_orient_matrix_UB_13      -0.0027113000
_diffrn_orient_matrix_UB_21      -0.0001896000
_diffrn_orient_matrix_UB_22      0.0010638000
_diffrn_orient_matrix_UB_23      -0.0306346000
_diffrn_orient_matrix_UB_31      0.0096913000
_diffrn_orient_matrix_UB_32      -0.0297154000
_diffrn_orient_matrix_UB_33      -0.0004031000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43524
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.733
_diffrn_reflns_theta_min         2.488
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80646
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       plate
_exptl_crystal_F_000             4962
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1416
_refine_ls_number_reflns         20622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0482P)^2^+21.3980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16548
_reflns_number_total             20622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00283e2.cif
_cod_data_source_block           kb2119
_cod_depositor_comments
'Adding full bibliography for 7045755--7045760.cif.'
_cod_database_code               7045760
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Co N6 C30 H30 C4 F12 S4 O8 N2'
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.833
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
  C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39), C40(H40),
 C41(H41), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28),
  C29(H29), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39),
 C40(H40), C41(H41), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C61(H61),
  C65(H65)
3.b Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C59(H59A,H59B,H59C)
;
_olex2_submission_special_instructions 'No special instructions were received'