A new chalcocyanide cubane rhenium salt: tetrakis(tetraphenylphosphonium) dodecacyano-<i>hexahedro</i>-tetratelluriumtetrarhenate(IV) trihydrate
Efremova, Olga A.; Mironov, Yuri V.; Kuratieva, Natalia V.; Fedorov, Vladimir E.; Acta Crystallographica Section E 60 (2004) m1817–m1818; doi:10.1107/S1600536804028454

data_2204692
_publ_section_title
;
 A new chalcocyanide cubane rhenium salt:
 tetrakis(tetraphenylphosphonium)
 dodecacyano-<i>hexahedro</i>-tetratelluriumtetrarhenate(IV) trihydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1817
_journal_page_last               m1818
_journal_paper_doi               10.1107/S1600536804028454
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C24 H20 P)4 [Re4 Te4 (C N)12], 3H2 O'
_chemical_formula_moiety         '4C24 H20 P +, C12 N12 Re4 Te4 4-, 3H2 O'
_chemical_formula_sum            'C108 H86 N12 O3 P4 Re4 Te4'
_chemical_formula_weight         2978.97
_chemical_name_systematic
;
tetrakis(tetraphenylphosphonium)
dodecacyano-hexahedro-tetratelluriumtetrarhenium(IV) trihydrate
;
_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_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                 105.1810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4635(8)
_cell_length_b                   24.1703(11)
_cell_length_c                   28.5358(11)
_cell_measurement_reflns_used    3070
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.51
_cell_measurement_theta_min      2.24
_cell_volume                     10293.3(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker--Nonius X8Apex CCD'
_diffrn_measurement_method       \f
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76502
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.919
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.565
_refine_diff_density_min         -1.242
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1216
_refine_ls_number_reflns         25536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0331P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                11085
_reflns_number_total             25536
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6116.cif
_cod_data_source_block           III
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (30 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (30 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2204692
_cod_database_fobs_code          2204692