Ag29(BDT)12(TPP)4: A Tetravalent Nanocluster.
AbdulHalim, Lina G.; Bootharaju, Megalamane S.; Tang, Qing; Del Gobbo, Silvano; AbdulHalim, Rasha G.; Eddaoudi, Mohamed; Jiang, De-En; Bakr, Osman M.; Journal of the American Chemical Society 137 (2015) 11970–11975; doi:10.1021/jacs.5b04547

data_4123925
_publ_section_title
;
 Ag29(BDT)12(TPP)4: A Tetravalent Nanocluster.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11970
_journal_page_last               11975
_journal_paper_doi               10.1021/jacs.5b04547
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C144 H108 Ag29 P4 S24'
_chemical_formula_sum            'C165 H157 Ag29 N7 O7 P4 S24'
_chemical_formula_weight         6371.52
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.08 svn.r3125 for OlexSys, GUI svn.r3563)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.2011(8)
_cell_length_b                   34.2011(8)
_cell_length_c                   34.2011(8)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.000
_cell_measurement_theta_min      0.000
_cell_volume                     40005.5(16)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1367
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84881
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        44.850
_diffrn_reflns_theta_max         44.850
_diffrn_reflns_theta_min         5.332
_exptl_absorpt_coefficient_mu    25.214
_exptl_absorpt_correction_T_max  0.6455
_exptl_absorpt_correction_T_min  0.5226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1008 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.8096. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_description       plate
_exptl_crystal_F_000             24472
_exptl_crystal_recrystallization_method
'The material was recrystallised from DMF by slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.0894
_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^)+(0.0716P)^2^+2996.1311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3196
_reflns_number_total             5330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04547_si_002.cif
_cod_data_source_block           kme_910_0m_sq
_cod_depositor_comments          'Adding full bibliography for 4123925.cif.'
_cod_original_cell_volume        40006(3)
_cod_database_code               4123925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 Ag1, Ag2, Ag3, Ag4, Ag5, Ag21, Ag24, Ag31, Ag41, Ag51, Ag55, S2, S3, S4, S5,
 S22, S34, S35, S45, P24, P55, C20, C21, C22, H22, C23, H23, C24, C25, H25, C30,
  C31, H31, C32, H32, C33, H33, C34, C35, H35, C40, C41, H41, C42, H42, C43,
 H43, C44, C45, H45, C50, C51, H51, C52, C53, H53, C54, H54, C55, H55, C240,
 C241, H241, C242, H242, C243, H243, C244, H244, C245, H245, C246, C247, H247,
 C248, H248, C249, H249, C250, H250, C251, H251, C252, C253, H253, C254, H254,
 C255, H255, C256, H256, C257, H257, C551, C552, H552, C553, H553, C554, H554,
 C555, H555, C556, H556
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C25(H25), C31(H31), C32(H32), C33(H33),
 C35(H35), C45(H45), C43(H43), C42(H42), C41(H41), C51(H51), C53(H53), C54(H54),
  C55(H55), C245(H245), C244(H244), C243(H243), C242(H242), C241(H241),
 C247(H247), C248(H248), C249(H249), C250(H250), C251(H251), C257(H257),
 C256(H256), C255(H255), C254(H254), C253(H253), C556(H556), C555(H555),
 C554(H554), C553(H553), C552(H552)
3.b Fitted hexagon refined as free rotating group:
 C20(C21,C22,C23,C24,C25), C40(C45,C44,C43,C42,C41), C240(C245,C244,C243,C242,
 C241), C246(C247,C248,C249,C250,C251), C252(C257,C256,C255,C254,C253),
 C551(C556,C555,C554,C553,C552)
;
_shelx_fab_checksum              68362
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2015-01-05
_olex2_date_sample_data_collection 2015-01-04
_olex2_date_sample_submission    2015-01-04
_olex2_submission_special_instructions 'No special instructions were received'