Synthesis and Structural Characterization of an Unusual Oxygen-Linked Double Cubane-Like Cluster {[Mo3PbOS3](OAc)2(py)3(dtp)2O}2
Rong-Min Yu; Shao-Fang Lu; Xiao-Ying Huang; Qiang-Jin Wu; Jian-Quan Huang; Inorganic Chemistry 38 (1999) 3313–3315; doi:10.1021/ic9703890

data_4322122
_publ_section_title
;
 Synthesis and Structural Characterization of an Unusual Oxygen-Linked
 Double Cubane-Like Cluster {[Mo3PbOS3](OAc)2(py)3(dtp)2O}2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3313
_journal_page_last               3315
_journal_paper_doi               10.1021/ic9703890
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'Pb2 Mo6 S14 P4 O20 N6 C54 H82'
_chemical_formula_sum            'C54 H82 Mo6 N6 O20 P4 Pb2 S14'
_chemical_formula_weight         2698.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source
'International Tables for X-Ray Crystallography Vol.IV '
_audit_creation_date             30-SEP-97
_audit_creation_method           from_GCIF_by_our_laboratory
_cell_angle_alpha                90
_cell_angle_beta                 98.14(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.705(8)
_cell_length_b                   19.527(8)
_cell_length_c                   20.670(9)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     4677(4)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'Lorentz-Polarization (MolEN)'
_computing_molecular_graphics    'ORTEP (1989)'
_computing_publication_material  GCIF_by_Our_laboratory
_computing_structure_refinement  'Full Matrix Least Squares-LSFM (MolEN)'
_computing_structure_solution    'Patterson (MolEN)'
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8900
_diffrn_reflns_theta_max         25.0
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.80
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   empirical_\y
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.92
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.74
_refine_diff_density_min         -0.24
_refine_ls_goodness_of_fit_obs   0.86
_refine_ls_hydrogen_treatment    'Not Refined'
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5424
_refine_ls_R_factor_obs          .0564
_refine_ls_shift/esd_max         0.0118
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(F)+(.020F)^2^+1.0]-F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .0682
_reflns_number_observed          5424
_reflns_number_total             8480
_reflns_observed_criterion       refl_observed_if_I_>3.0_sigma(I)
_cod_data_source_file            ic9703890.cif
_cod_data_source_block           IC9703890
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (65 times).

'_geom_angle_publ_flag' value
'Yes' changed to 'yes' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (156
times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/[\s^2^(F)+(.020F)^2^+1.0]-F'
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^(F)+(.020F)^2^+1.0]-F'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4677(8)
_cod_original_formula_sum        'Pb2 Mo6 S14 P4 O20 N6 C54 H82'
_cod_database_code               4322122