Complete Ag4M2(DMSA)4 (M = Ni, Pd, Pt, DMSA = Dimercaptosuccinic Acid) Cluster Series: Optical Properties, Stability, and Structural Characterization.
Biltek, Scott R.; Reber, Arthur C.; Khanna, Shiv N.; Sen, Ayusman; The journal of physical chemistry. A 121 (2017) 5324–5331; doi:10.1021/acs.jpca.7b04669

data_1547524
_publ_section_title
;
 Complete Ag4M2(DMSA)4 (M = Ni, Pd, Pt, DMSA = Dimercaptosuccinic Acid)
 Cluster Series: Optical Properties, Stability, and Structural
 Characterization.
;
_journal_issue                   28
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              5324
_journal_page_last               5331
_journal_paper_doi               10.1021/acs.jpca.7b04669
_journal_volume                  121
_journal_year                    2017
_chemical_formula_moiety
'C16 H16 Ag4 Ni2 O16 S8, C4 H9 N O3, C2.78 H5.48 N0.7 O2.7, 10.38(Na0.67), 14(O)'
_chemical_formula_sum            'C22.78 H30.48 Ag4 N1.7 Na6.96 Ni2 O35.69 S8'
_chemical_formula_weight         1864.60
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.054(5)
_cell_length_b                   17.452(4)
_cell_length_c                   26.296(6)
_cell_measurement_reflns_used    8622
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.288
_cell_measurement_theta_min      2.243
_cell_volume                     11498(4)
_computing_cell_refinement       'SAINT V6.36A (BRUKER, 2016)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.36A (BRUKER, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            103984
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           32.0
_diffrn_source_power             1.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.7942
_exptl_absorpt_correction_T_min  0.176217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.05 (BRUKER, 2001) was used for absorption correction.
R(int) was 0.0604 before and 0.0289 after correction.
The Ratio of minimum to maximum transmission is 0.1762.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7305
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.584
_refine_diff_density_min         -3.297
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         14245
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.1020
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+394.1211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2384
_reflns_number_gt                11249
_reflns_number_total             14245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp7b04669_si_002.cif
_cod_data_source_block           srb3o
_cod_original_formula_sum
'C22.78 H30.48 Ag4 N1.70 Na6.96 Ni2 O35.69 S8'
_cod_database_code               1547524
_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 O(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
4. Same fragment restrains
{C1, C2, C3, C4} sigma for 1-2: 0.02, 1-3: 0.04
as
{C5, C6, C7, C8}
{C17, C18, C19, C20, N1, O17, O18, O19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C21, C22, C23, C24, N2, O20, O21, O22}
5. Others
 Sof(Na8)=1-FVAR(1)
 Sof(C21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(N2)=Sof(O22)=Sof(H22)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4), O6(H6A), O7(H7A), O10(H10A), O11(H11A), O13(H13), O15(H15A),
 O17(H17), O18(H18), O19(H19), O20(H20), O21(H21), O22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'