Synthesis, Structure, and Properties of Molybdenum and Tungsten Cyano Complexes with Cuboidal M4(μ3-E4) (M = Mo, W; E = S, Se, Te) Cores
V. P. Fedin; I. V. Kalinina; D. G. Samsonenko; Y. V. Mironov; M. N. Sokolov; S. V. Tkachev; A. V. Virovets; N. V. Podberezskaya; M. R. J. Elsegood; W. Clegg; A. G. Sykes; Inorganic Chemistry 38 (1999) 1956–1965; doi:10.1021/ic980956z

data_4321941
_publ_section_title
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 Synthesis, Structure, and Properties of Molybdenum and Tungsten Cyano
 Complexes with Cuboidal M4(\m3-E4) (M = Mo, W; E = S, Se, Te) Cores
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1956
_journal_page_last               1965
_journal_paper_doi               10.1021/ic980956z
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C13 H8 Cs5 K N12 O3 S4 W4'
_chemical_formula_weight         1947.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'H-atoms not included'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.568(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.116(4)
_cell_length_b                   10.335(3)
_cell_length_c                   19.414(5)
_cell_measurement_reflns_used    12990
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.23
_cell_volume                     3617.7(16)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.859
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22572
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.019
_exptl_absorpt_correction_T_max  0.335
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.401
_refine_diff_density_min         -3.572
_refine_diff_density_rms         0.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                6051
_reflns_number_total             8519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980956z_1.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0392P)^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^)+(0.0392P)^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_cell_volume        3617.7(15)
_cod_database_code               4321941