Chemistry in Environmentally Benign Media. 3.1 Synthesis and Characterization of Rhenium(V) Complexes Derived from Novel Water-Soluble (Hydroxymethyl)phosphines. Crystal Structures of [Re(O)2{(HOH2C)2PC6H4P(CH2OH)2}2]I and [Re(O)2{(HOH2C)2PCH2CH2P(CH2OH)2}2]Cl
V. Sreenivasa Reddy; Douglas E. Berning; Kattesh Katti; Charles L. Barnes; Wynn A. Volkert; A.R. Kettring; Inorganic Chemistry 35 (1996) 1753–1757; doi:10.1021/ic9510167

data_4324059
_publ_contact_author
;
Kattesh V. Katti
Center for Radiological Research and MURR
University of Missouri
Columbia, MO 65211
;
_publ_section_title
;
 Chemistry in Environmentally Benign Media. 3.1 Synthesis and
 Characterization of Rhenium(V) Complexes Derived from Novel Water-Soluble
 (Hydroxymethyl)phosphines. Crystal Structures of
 [Re(O)2{(HOH2C)2PC6H4P(CH2OH)2}2]I and
 [Re(O)2{(HOH2C)2PCH2CH2P(CH2OH)2}2]Cl
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1753
_journal_page_last               1757
_journal_paper_doi               10.1021/ic9510167
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         'C20 H32 O10 P4 Re I '
_chemical_formula_sum            'C20 H32 I O10 P4 Re'
_chemical_formula_weight         869.47
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 105.929(9)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   23.906(5)
_cell_length_b                   7.0493(6)
_cell_length_c                   17.024(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15.00
_cell_measurement_theta_min      10.00
_cell_volume                     2758.7(9)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Theta/2theta scan b/P/b '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2554
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.74
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             1674.18
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.35
_refine_diff_density_min         -1.04
_refine_ls_goodness_of_fit_obs   1.21
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2280
_refine_ls_R_factor_all          0.019
_refine_ls_R_factor_obs          0.019
_refine_ls_shift/esd_max         0.011
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(\s^2^(F)+0.0003F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.027
_refine_ls_wR_factor_obs         0.027
_reflns_number_observed          2280
_reflns_number_total             2421
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            ic9510167_1.cif
_cod_data_source_block           C20H32O10P4ReI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+0.0003F^2^)' 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^(F)+0.0003F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C20 H32 O10 P4 Re I '
_cod_database_code               4324059