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_7044163
_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         '1.5(C30 H48 Co N12), 3(C H3 O3 S)'
_chemical_formula_sum            'C48 H81 Co1.5 N18 O9 S3'
_chemical_formula_weight         1238.88
_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
_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                 112.358(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6765(7)
_cell_length_b                   12.9804(4)
_cell_length_c                   21.7673(7)
_cell_measurement_reflns_used    13046
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      29.1210
_cell_measurement_theta_min      3.1750
_cell_volume                     6186.9(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      99.9(2)
_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 -47.00 48.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -16.9951 77.0000 -180.0000 95 #__ type_ start__ end____ width___ exp.time_ 2 omega -11.00 65.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 0.0000 76 #__ type_ start__ end____ width___ exp.time_ 3 omega 12.00 80.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 60.0000 68'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0290610000
_diffrn_orient_matrix_UB_12      0.0176018000
_diffrn_orient_matrix_UB_13      0.0022414000
_diffrn_orient_matrix_UB_21      -0.0104504000
_diffrn_orient_matrix_UB_22      0.0516783000
_diffrn_orient_matrix_UB_23      -0.0028504000
_diffrn_orient_matrix_UB_31      0.0097560000
_diffrn_orient_matrix_UB_32      0.0030250000
_diffrn_orient_matrix_UB_33      0.0350700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28716
_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         26.372
_diffrn_reflns_theta_min         2.754
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78673
_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    1.330
_exptl_crystal_description       needle
_exptl_crystal_F_000             2622
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         12644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0348P)^2^+5.2880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10677
_reflns_number_total             12644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02604h2.cif
_cod_data_source_block           kb2103
_cod_original_cell_volume        6186.8(4)
_cod_original_formula_sum        'C48 H81 Co1.50 N18 O9 S3'
_cod_database_code               7044163
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Co C4 F12 S4 O8 N2 N12 C36 H56'
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.803
_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) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(S76A)=Sof(O77A)=Sof(H80D)=Sof(H80E)=Sof(H80F)=1-FVAR(1)
 Sof(S76)=Sof(O77)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B), C28(H28A,H28B), C34(H34A,H34B), C40(H40A,
 H40B), C46(H46A,H46B), C52(H52A,H52B), C58(H58A,H58B), C64(H64A,H64B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C18(H18), C20(H20), C21(H21), C24(H24),
 C26(H26), C27(H27), C30(H30), C32(H32), C33(H33), C36(H36), C38(H38), C39(H39),
  C42(H42), C44(H44), C45(H45), C48(H48), C50(H50), C51(H51), C54(H54),
 C56(H56), C57(H57), C60(H60), C62(H62), C63(H63)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C35(H35A,H35B,
 H35C), C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C59(H59A,
 H59B,H59C), C65(H65A,H65B,H65C), C70(H70A,H70B,H70C), C75(H75A,H75B,H75C),
 C80(H80A,H80B,H80C), C80(H80D,H80E,H80F)
;
_shelx_res_checksum              7602
_olex2_submission_special_instructions 'No special instructions were received'