Formation (and properties) of palladium derivatives of [Mo3Q4(H2O)9]4+: absence of similar derivatives of [W3Q4(H2O)9]4+ (Q = S, Se)
Vladimir P. Fedin; Mi-Sook Seo; David M. Saysell; Danil N. Dybtsev; Mark R. J. Elsegood; William Clegg; A. Geoffrey Sykes; J. Chem. Soc., Dalton Trans.  (2002) 138–143; doi:10.1039/b106522j

data_7010993
_publ_section_title
;
 Formation (and properties) of palladium derivatives of
 [Mo3Q4(H2O)9]4+: absence of similar derivatives of [W3Q4(H2O)9]4+ (Q =
 S, Se)
;
_journal_issue                   2
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              138
_journal_page_last               143
_journal_paper_doi               10.1039/b106522j
_journal_year                    2002
_chemical_formula_sum            'C28 H64 Mo3 O30 Pd S4 Se4'
_chemical_formula_weight         1719.09
_chemical_name_systematic
;
?
;
_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                77.380(2)
_cell_angle_beta                 84.506(3)
_cell_angle_gamma                82.822(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6971(11)
_cell_length_b                   14.9372(15)
_cell_length_c                   16.4307(16)
_cell_measurement_reflns_used    14649
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      2.25
_cell_volume                     2772.5(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20783
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.842
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.810
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         12534
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                9739
_reflns_number_total             12534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106522j.txt
_cod_data_source_block           ags27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010993