Cyclodiphosphazanes with Hemilabile Ponytails: Synthesis, Transition Metal Chemistry (Ru(II), Rh(I), Pd(II), Pt(II)), and Crystal and Molecular Structures of Mononuclear (Pd(II), Rh(I)) and Bi- and Tetranuclear Rhodium(I) Complexes
P. Chandrasekaran; Joel T. Mague; Maravanji S. Balakrishna; Inorganic Chemistry 44 (2005) 7925–7932; doi:10.1021/ic0509478

data_4309873
_publ_section_title
;
Cyclodiphosphazanes with Hemilabile Ponytails: Synthesis, Transition
Metal Chemistry (Ru(II), Rh(I), Pd(II), Pt(II)), and Crystal and Molecular
Structures of Mononuclear (Pd(II), Rh(I)) and Bi- and Tetranuclear
Rhodium(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7925
_journal_page_last               7932
_journal_paper_doi               10.1021/ic0509478
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C16 H32 Cl2 N2 O6 P2 Rh2'
_chemical_formula_sum            'C16 H32 Cl2 N2 O6 P2 Rh2'
_chemical_formula_weight         687.10
_chemical_name_systematic
; 
 Tetra(\m-chloro)tetracarbonylbis(\m-(1,3-di-tert
-butyl-2,4-bis(2-methoxyethoxy)-[1,3,2,4]
diazadiphosphetidine,\k,P;\k,P)tetrarhodium(I)
;
_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                 99.753(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3390(9)
_cell_length_b                   18.286(2)
_cell_length_c                   14.916(1)
_cell_measurement_reflns_used    7050
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.62
_cell_volume                     2510.4(4)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2002)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'BRUKER-AXS 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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21656
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.8726
_exptl_absorpt_correction_T_min  0.7208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5749
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0424P)^2^+4.1258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                5139
_reflns_number_total             5749
_reflns_threshold_expression     >2\sw(I)
_cod_data_source_file            ic0509478si20050611_094104.cif
_cod_data_source_block           msb165
_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.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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_database_code               4309873