Heterobimetallic Lantern Complexes That Couple Antiferromagnetically through Noncovalent Pt...Pt Interactions
Frederick G. Baddour; Stephanie R. Fiedler; Matthew P. Shores; James A. Golen; Arnold L. Rheingold; Linda H. Doerrer; Inorganic Chemistry 52 (2013) 4926–4933; doi:10.1021/ic302531t

data_4334599
_publ_section_title
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 Heterobimetallic Lantern Complexes That Couple Antiferromagnetically
 through Noncovalent Pt...Pt Interactions
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4926
_journal_page_last               4933
_journal_paper_doi               10.1021/ic302531t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C8 H18 Co O7 Pt S4'
_chemical_formula_weight         608.48
_chemical_name_systematic
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 ? 
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_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.951(3)
_cell_angle_beta                 88.436(3)
_cell_angle_gamma                87.007(3)
_cell_formula_units_Z            4
_cell_length_a                   8.3411(7)
_cell_length_b                   14.1061(12)
_cell_length_c                   16.1443(14)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.45
_cell_volume                     1745.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'doubly curved mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23375
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    9.457
_exptl_absorpt_correction_T_max  0.7035
_exptl_absorpt_correction_T_min  0.4514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.4356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0519
_reflns_number_gt                6228
_reflns_number_total             6999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302531t_si_002_1.cif
_cod_data_source_block           lhd318_compound1_PtMSAcdimers
_cod_database_code               4334599
_comment_alert_responses
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B level alerts (2_B), (4_B) were generated and are attributed to short O-H and 
H-C interactions and long hydrogen bonds of 1.9-2 are included in the listing 
for future studies. There was residual electron density found close to Pt and 
S, but no attempt was made to model this density.
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_alert_c_comments_reply_lhd324
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DIFX01 and DIF02  - Electron density within 1.1 angstroms of Pt atoms.

PLAT094  Alert C ratio of max/min electron density is large.

Reply  density found within 1.1. angstroms of Pt atoms.

Plat097  Alert C Large positive residual electron density.

Crystals of sample LHD324 were thin plates and no absorption correction other 
than SADABS was made. Refinment exhibits  high esu values, large number of 
residual electron density peaks, and high weight refinement value indicative 
of possible absorption issues.  Highest electron density peaks were found with 
1.1 angstroms of Pt1 and Pt2.  Attempts to treat residual electron density as 
satellites of Pt were not successful.
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