New Rhodium(III) and Ruthenium(II) Water-Soluble Complexes with 3,5-Diaza-1-methyl-1-azonia-7-phosphatricyclo[3.3.1.13,7]decane
Piotr Smoleński; Florian P. Pruchnik; Zbigniew Ciunik; Tadeusz Lis; Inorganic Chemistry 42 (2003) 3318–3322; doi:10.1021/ic034044v

data_4313664
_publ_contact_author
;
Florian P. Pruchnik
Faculty of Chemistry, University of Wroclaw,
14. F. Joliot-Curie Street, 50-383 Wroclaw,
Poland
;
_publ_contact_author_email       pruchnik@wchuwr.chem.uni.wroc.pl
_publ_section_title
;
 New Rhodium(III) and Ruthenium(II) Water-Soluble Complexes with
 3,5-Diaza-1-methyl-1-azonia-7-phosphatricyclo[3.3.1.13,7]decane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3318
_journal_page_last               3322
_journal_paper_doi               10.1021/ic034044v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[RuI2{P(CH2)6N2NCH3}3(H2O)]I3.2H2O'
_chemical_formula_sum            'C21 H51 I5 N9 O3 P3 Ru'
_chemical_formula_weight         1306.19
_chemical_name_common
;
aquatris{diazamethylazoniaphosphaadamantane}
-diiodoruthenium(II)triiodide dihydrate
;
_chemical_name_systematic
;
    (OC-6-13)-aqua{tris(3,5-diaza-1-methyl-1-azonia-7
    -phosphatricyclo[3.3.1.1^3,7]decane}diiodoruthenium(II)
    -triiodide-water (1/2)
;
_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                 92.824(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6234(11)
_cell_length_b                   15.3353(9)
_cell_length_c                   18.1723(12)
_cell_measurement_reflns_used    3200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      3.28
_cell_volume                     3791.9(5)
_computing_cell_refinement       'Oxford Diffraction (Poland) Sp. z o.o'
_computing_data_collection       'Oxford Diffraction (Poland) Sp. z o.o'
_computing_data_reduction        'Oxford Diffraction (Poland) Sp. z o.o'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25592
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         3.28
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    4.649
_exptl_absorpt_correction_type   |Fo|-|Fc|
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                7428
_reflns_number_total             8911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034044vsi20030326_081136_3.cif
_cod_data_source_block           sm3abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313664
_exptl_absorpt_correction_a_min  0.73269
_exptl_absorpt_correction_a_max  1.51202