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_4321945
_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_moiety         'K7 (Mo4 Te4 (C N)12) . (H2 O)12'
_chemical_formula_sum            'C12 H24 K7 Mo4 N12 O12 Te4'
_chemical_formula_weight         1696.29
_chemical_name_systematic
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 ?
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_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.112(1)
_cell_length_b                   21.736(2)
_cell_length_c                   16.109(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      10.0
_cell_volume                     4241.0(6)
_computing_cell_refinement       CD4CA0
_computing_data_collection       CD4CA0
_computing_data_reduction        CADDAT
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5874
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '3600 sec'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.600
_exptl_absorpt_correction_T_max  1.3364
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   '5 psi scans'
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3140
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.00025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          2.363
_refine_ls_shift/su_mean         0.101
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+10.9232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                4707
_reflns_number_total             5874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980956z_5.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321945