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_7045756
_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         'C30 H54 Co N6 O6, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C34 H54 Co F12 N8 O14 S4'
_chemical_formula_weight         1214.02
_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             2017-09-08
_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                92.887(3)
_cell_angle_beta                 100.337(3)
_cell_angle_gamma                107.217(4)
_cell_formula_units_Z            2
_cell_length_a                   13.2653(5)
_cell_length_b                   14.2526(6)
_cell_length_c                   14.3590(5)
_cell_measurement_reflns_used    9190
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9940
_cell_measurement_theta_min      3.2420
_cell_volume                     2535.53(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      100.00(10)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 7.00 88.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 57.0000 90.0000 81 #__ type_ start__ end____ width___ exp.time_ 2 omega -3.00 46.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 57.0000 -180.0000 49 #__ type_ start__ end____ width___ exp.time_ 3 omega -8.00 79.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 -120.0000 87 #__ type_ start__ end____ width___ exp.time_ 4 omega -38.00 8.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 -57.0000 -180.0000 46 #__ type_ start__ end____ width___ exp.time_ 5 omega -51.00 49.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 -77.0000 -30.0000 100'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0406298000
_diffrn_orient_matrix_UB_12      0.0238568000
_diffrn_orient_matrix_UB_13      -0.0246223000
_diffrn_orient_matrix_UB_21      -0.0036935000
_diffrn_orient_matrix_UB_22      -0.0463811000
_diffrn_orient_matrix_UB_23      -0.0231951000
_diffrn_orient_matrix_UB_31      -0.0400608000
_diffrn_orient_matrix_UB_32      0.0052441000
_diffrn_orient_matrix_UB_33      -0.0375233000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18375
_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         26.370
_diffrn_reflns_theta_min         2.902
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80950
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1250
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         10355
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0286P)^2^+2.7719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9049
_reflns_number_total             10355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00283e2.cif
_cod_data_source_block           kb2076
_cod_depositor_comments
'Adding full bibliography for 7045755--7045760.cif.'
_cod_original_cell_volume        2535.52(18)
_cod_database_code               7045756
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Co C4 F12 N2 S4 O8 N6 O6 C30 H56'
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.887
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C59-F61 = C59-F62 = C59-F63 = C60-F64 = C60-F65 = C60-F66
 1.321 with sigma of 0.005
 C74-F75 = C74-F76 = C74-F77 = C74-F78 = C74-F79 = C74-F80
 1.321 with sigma of 0.005
 C87-F88 = C87-F89 = C87-F90 = C91-F92 = C91-F93 = C91-F94
 1.321 with sigma of 0.005
3. Rigid body (RIGU) restrains
 F50, F51, F52, F61, F62, F63, S56, O57, O58, C60, F64, F65, F66, F75, F76,
 F77, F78, F79, F80, F88, F89, F90, F92, F93, F94
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(N45)=Sof(S56)=Sof(O57)=Sof(O58)=Sof(C60)=Sof(F64)=Sof(F65)=Sof(F66)=1-
 FVAR(1)
 Sof(N44)=Sof(S53)=Sof(O54)=Sof(O55)=Sof(C59)=Sof(F61)=Sof(F62)=Sof(F63)=FVAR(1)
 Sof(F78)=Sof(F79)=Sof(F80)=1-FVAR(2)
 Sof(F75)=Sof(F76)=Sof(F77)=FVAR(2)
 Sof(C91)=Sof(F92)=Sof(F93)=Sof(F94)=1-FVAR(3)
 Sof(C87)=Sof(F88)=Sof(F89)=Sof(F90)=FVAR(3)
 Fixed Sof: N67(0.5) S68(0.5) O69(0.5) O70(0.5) S71(0.5) O72(0.5) O73(0.5)
 N81(0.5) S82(0.5) O83(0.5) S84(0.5) O85(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C31(H31A,H31B,
 H31C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              78102
_olex2_submission_special_instructions 'No special instructions were received'