Group 11 Complexes of the P,Te-Centered Ligand [TePiPr2NPiPr2]-: Synthesis, Structures, and Insertion Reactions of the Copper(I) Complex with Chalcogens
Jamie S. Ritch; Tristram Chivers; Inorganic Chemistry 48 (2009) 3857–3865; doi:10.1021/ic802428b

data_4301995
_publ_section_title
;
Group 11 Complexes of the P,Te-Centered Ligand [TePiPr2NPiPr2]-:
Synthesis, Structures, and Insertion Reactions of the Copper(I) Complex
with Chalcogens
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3857
_journal_page_last               3865
_journal_paper_doi               10.1021/ic802428b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C36 H84 Cu2 N3 P6 Se3 Te3'
_chemical_formula_sum            'C36 H84 Cu2 N3 P6 Se3 Te3'
_chemical_formula_weight         1555.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                117.27(3)
_cell_angle_beta                 95.65(3)
_cell_angle_gamma                91.29(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4684(17)
_cell_length_b                   20.421(4)
_cell_length_c                   21.183(4)
_cell_measurement_reflns_used    58788
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.25
_cell_volume                     3230.8(14)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi\omega scans'
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            58788
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.168
_exptl_absorpt_correction_T_max  0.8510
_exptl_absorpt_correction_T_min  0.4894
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
; 
A heavily disordered hexane molecule was present in the asymmetric unit, 
however no suitable model for refinement could be found. SQUEEZE was 
used to remove the reflection data associated with this molecule, 
leaving a void in the unit cell of ca. 445 cubic Angstroms.
;
_refine_diff_density_max         2.472
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         14646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.4364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                9965
_reflns_number_total             14646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802428b_si_001_6.cif
_cod_data_source_block           compound11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4301995