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_7044164
_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         '2(C18 H30 Co0.5 N6), 2(C H3 O3 S)'
_chemical_formula_sum            'C38 H66 Co N12 O6 S2'
_chemical_formula_weight         910.07
_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             2016-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3353 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-04-24 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                88.763(3)
_cell_angle_beta                 80.229(3)
_cell_angle_gamma                85.243(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8446(3)
_cell_length_b                   15.7075(6)
_cell_length_c                   17.6599(7)
_cell_measurement_reflns_used    6531
_cell_measurement_temperature    250.01(10)
_cell_measurement_theta_max      27.0750
_cell_measurement_theta_min      3.0310
_cell_volume                     2409.44(16)
_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      250.01(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
;
  1 omega  -39.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   38.0000  -90.0000 33

  2 omega  -87.00   12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -77.0000    0.0000 99

  3 omega  -86.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -57.0000  120.0000 83

  4 omega  -69.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -57.0000   30.0000 66

  5 omega  -87.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951  -77.0000 -120.0000 92

  6 omega   49.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000  -60.0000 35
;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Eos detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0672907000
_diffrn_orient_matrix_UB_12      0.0246368000
_diffrn_orient_matrix_UB_13      -0.0068878000
_diffrn_orient_matrix_UB_21      0.0347553000
_diffrn_orient_matrix_UB_22      0.0062296000
_diffrn_orient_matrix_UB_23      -0.0387523000
_diffrn_orient_matrix_UB_31      -0.0304841000
_diffrn_orient_matrix_UB_32      -0.0375179000
_diffrn_orient_matrix_UB_33      -0.0105807000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19415
_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         2.791
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74008
_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    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0874P)^2^+2.0757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7292
_reflns_number_total             9822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02604h2.cif
_cod_data_source_block           kb2102-vt_3_250_00
_cod_database_code               7044164
_chemical_oxdiff_formula         'Co C4 F12 S4 O8 N2 N12 C36 H56'
_reflns_odcompleteness_completeness 84.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C14-C15 = C14A-C15A
 1.5 with sigma of 0.005
 C13-C15 = C13-C15A
 2.5 with sigma of 0.005
 C13-C14 = C13-C14A
 1.42 with sigma of 0.005
 S51-O52 = S51A-O52A = S51-O53 = S51A-O53A = S51-O54 = S51A-O54
 1.4 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C14A \\sim C15A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{N17, C18, C19, C20, C21, C22} sigma for 1-2: 0.01, 1-3: 0.02
as
{N24, C25, C26, C27, C28, C29}
{N17, C18, C19, C20, C21, C22} sigma for 1-2: 0.01, 1-3: 0.02
as
{N31, C32, C33, C34, C35, C36}
{N17, C18, C19, C20, C21, C22} sigma for 1-2: 0.01, 1-3: 0.02
as
{N38, C39, C40, C41, C42, C43}
6. Others
 Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C50A)=
 Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(1)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=
 Sof(H50B)=Sof(H50C)=FVAR(1)
 Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=1-FVAR(2)
 Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=FVAR(2)
 Sof(S51A)=Sof(O52A)=Sof(O53A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=1-FVAR(3)
 Sof(S51)=Sof(O52)=Sof(O53)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13(H13C,H13D), C14(H14A,H14B), C14A(H14C,H14D), C20(H20A,
 H20B), C21(H21A,H21B), C27(H27A,H27B), C28(H28A,H28B), C34(H34A,H34B),
 C35(H35A,H35B), C41(H41A,H41B), C42(H42A,H42B), C48(H48A,H48B), C48A(H48C,
 H48D), C49(H49A,H49B), C49A(H49C,H49D)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C12(H12), C16(H16), C18(H18), C19(H19), C23(H23), C25(H25),
 C26(H26), C30(H30), C32(H32), C33(H33), C37(H37), C39(H39), C40(H40), C44(H44),
  C46(H46), C47(H47)
7.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C22(H22A,H22B,H22C), C29(H29A,H29B,
 H29C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C),
 C50A(H50D,H50E,H50F), C55(H55A,H55B,H55C), C55(H55D,H55E,H55F), C60(H60A,H60B,
 H60C)
;
_shelx_res_checksum              54544
_shelx_shelxl_version_number     2016/4
_olex2_date_sample_data_collection 2015-01-28
_olex2_submission_special_instructions 'No special instructions were received'