An Acyclic Dimer of Cyclodiphosphazane {tBuHN(tBuNP)2OCH2}2 Containing Alkoxo and Amido Functionalities: Synthesis, Derivatization, Bi- (PdII, RhI), and Tetranuclear (PdII, AuI, RhIAuI) Transition Metal Complexes
Maravanji S. Balakrishna; Ramalingam Venkateswaran; Joel T. Mague; Inorganic Chemistry 48 (2009) 1398–1406; doi:10.1021/ic801256h

data_4301413
_publ_section_title
;
An Acyclic Dimer of Cyclodiphosphazane {tBuHN(tBuNP)2OCH2}2 Containing
Alkoxo and Amido Functionalities: Synthesis, Derivatization, Bi- (PdII,
RhI), and Tetranuclear (PdII, AuI, RhIAuI) Transition Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1398
_journal_page_last               1406
_journal_paper_doi               10.1021/ic801256h
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C26 H60 Au4 Cl4 N6 O2 P4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C26.5 H61 Au4 Cl5 N6 O2 P4'
_chemical_formula_weight         1584.81
_chemical_name_systematic
; 
 Tetrachloro-1\k,2\k,3\k,4\k-\m(1,2-Bis(1,3-di-tert-butyl-4-
tert-butylamino[1,3,2,4]diazadiphosphetidin-2-oxy)ethane-1\k
P:2\kP':3\kP":4\kP'")tetragold(I) 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.775(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.783(1)
_cell_length_b                   18.779(2)
_cell_length_c                   14.044(2)
_cell_measurement_reflns_used    7690
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.41
_cell_volume                     2494.8(5)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43880
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    12.150
_exptl_absorpt_correction_T_max  0.4044
_exptl_absorpt_correction_T_min  0.1182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.750
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         12248
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                10769
_reflns_number_total             12248
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic801256h_si_002_5.cif
_cod_data_source_block           msb276a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C26.50 H61 Au4 Cl5 N6 O2 P4'
_cod_database_code               4301413
_cod_duplicate_entry 4301405