Synthesis and Structure of [PPh4]3[Cr(Te4)3].DMF: The First Tris(tetratelluride) Complex
Perumal Sekar; James A. Ibers; Inorganic Chemistry 41 (2002) 450–451; doi:10.1021/ic015585s

data_4317525
_publ_section_title
;
 Synthesis and Structure of [PPh4]3[Cr(Te4)3].DMF: The First
 Tris(tetratelluride) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              450
_journal_page_last               451
_journal_paper_doi               10.1021/ic015585s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C75 H67 Cr N O P3 Te12'
_chemical_formula_weight         2674.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                90.63(3)
_cell_angle_beta                 104.45(3)
_cell_angle_gamma                106.49(3)
_cell_formula_units_Z            2
_cell_length_a                   12.991(3)
_cell_length_b                   14.782(3)
_cell_length_c                   24.628(5)
_cell_measurement_temperature    153(2)
_cell_volume                     4374.3(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40229
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    4.15
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2450
_refine_diff_density_max         2.696
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         20233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0474
_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 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                14447
_reflns_number_total             20233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015585s_s1.cif
_cod_data_source_block           crte
_cod_original_cell_volume        4374.2(15)
_cod_original_formula_sum        'C72 H60 Cr P3 Te12 .C3 H7 O N'
_cod_database_code               4317525