Atomically monodisperse nickel nanoclusters as highly active electrocatalysts for water oxidation.
Joya, Khurram S.; Sinatra, Lutfan; AbdulHalim, Lina G.; Joshi, Chakra P.; Hedhili, M. N.; Bakr, Osman M.; Hussain, Irshad; Nanoscale 8 (2016) 9695–9703; doi:10.1039/c6nr00709k

data_1543077
_publ_section_title
;
 Atomically monodisperse nickel nanoclusters as highly active
 electrocatalysts for water oxidation.
;
_journal_issue                   18
_journal_name_full               Nanoscale
_journal_page_first              9695
_journal_page_last               9703
_journal_paper_doi               10.1039/c6nr00709k
_journal_volume                  8
_journal_year                    2016
_chemical_formula_moiety         'C96 H108 Ni6 S12, 2(C H2 Cl2)'
_chemical_formula_sum            'C98 H112 Cl4 Ni6 S12'
_chemical_formula_weight         2168.65
_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
_audit_creation_date             2015-08-19
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.06.29 svn.r3191 for OlexSys, GUI svn.r3563)
;
_cell_angle_alpha                77.032(4)
_cell_angle_beta                 82.429(4)
_cell_angle_gamma                89.334(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1685(11)
_cell_length_b                   12.4485(12)
_cell_length_c                   18.1823(18)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.54
_cell_measurement_theta_min      3.94
_cell_volume                     2441.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.15
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23227
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        66.751
_diffrn_reflns_theta_max         66.751
_diffrn_reflns_theta_min         2.516
_exptl_absorpt_coefficient_mu    4.999
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0886 before and 0.0437 after correction.
The Ratio of minimum to maximum transmission is 0.8219.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.466
_refine_diff_density_min         -2.985
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8407
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0852P)^2^+7.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7717
_reflns_number_total             8407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nr00709k3.cif
_cod_data_source_block           ni6_0m
_cod_depositor_comments
'Adding full bibliography for 1543077--1543078.cif.'
_cod_database_code               1543077
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1_2-C1_2 = Cl2_2-C1_2
 1.771 with sigma of 0.01
 Cl1_2-Cl2_2
 2.916 with sigma of 0.03
 Cl1_1-C1_1 = Cl2_1-C1_1
 1.771 with sigma of 0.01
 Cl1_1-Cl2_1
 2.916 with sigma of 0.03
 Cl1_3-C1_3 = Cl2_3-C1_3
 1.771 with sigma of 0.01
 Cl1_3-Cl2_3
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Cl1_2 \\sim Cl2_2 \\sim C1_2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl1_1 \\sim Cl2_1 \\sim C1_1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl1_3 \\sim Cl2_3 \\sim C1_3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl2_1 \\sim Cl1_1 \\sim C1_1: within 2A with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Cl1_3 \\sim C1_3 \\sim Cl2_3: within 2A with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Cl2_2 \\sim Cl1_2 \\sim C1_2: within 2A with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
4. Rigid body (RIGU) restrains
 Cl1_2, Cl2_2, C1_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_2, Cl1_2, Cl2_2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Cl1_1, Cl2_1, C1_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1_3, Cl2_3, C1_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl1(0.15) Cl2(0.15) C1(0.15) H1A(0.15) H1B(0.15) Cl1(0.65)
 Cl2(0.65) C1(0.65) H1A(0.65) H1B(0.65) Cl1(0.2) Cl2(0.2) C1(0.2) H1A(0.2)
 H1B(0.2)
6.a Free rotating group:
 Cl1(Cl2,C1), Cl1(Cl2,C1), Cl1(Cl2,C1)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C23(H23A,H23B), C27(H27A,H27B), C30(H30A,
 H30B), C33(H33A,H33B), C36(H36A,H36B), C38(H38A,H38B), C42(H42A,H42B),
 C47(H47A,H47B), C102(H10A,H10B), C101(H10C,H10D), C1(H1A,H1B), C1(H1A,H1B),
 C1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
 C25(H25), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C39(H39),
  C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
 C49(H49), C51(H51), C52(H52), C53(H53), C57(H57), C59(H59), C69(H69), C77(H77)
;
_shelx_res_checksum              45458
_shelx_hkl_checksum              28798
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'