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_4313662
_publ_contact_author
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Florian P. Pruchnik
Faculty of Chemistry, University of Wroclaw,
14. F. Joliot-Curie Street, 50-383 Wroclaw,
Poland
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_publ_contact_author_email       pruchnik@wchuwr.chem.uni.wroc.pl
_publ_section_title
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 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
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_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         '[RhI4{P(CH2)6N2NCH3}2]I'
_chemical_formula_sum            'C14 H30 I5 N6 P2 Rh'
_chemical_formula_weight         1081.79
_chemical_name_common
'bis{diazamethylazoniaphosphaadamantane} tetraiodorhodium(III) iodide'
_chemical_name_systematic
; 
    (OC-6-11)-{bis(3,5-diaza-1-methyl-1-azonia-7
    -phosphatricyclo[3.3.1.1^3,7]decane}tetraiodo
    -rhodium(III) iodide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.803(3)
_cell_length_b                   9.295(3)
_cell_length_c                   13.786(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1376.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7535
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    6.360
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.244
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0270P)^2^+8.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                2898
_reflns_number_total             3182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034044vsi20030326_081136_1.cif
_cod_data_source_block           rhic
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+8.5000P] 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^)+(0.0270P)^2^+8.5000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4313662