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_4324060
_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         'C12 H32 O10 P4 Cl2 Re '
_chemical_formula_sum            'C12 H32 Cl2 O10 P4 Re'
_chemical_formula_weight         717.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                104.430(10)
_cell_angle_beta                 96.400(10)
_cell_angle_gamma                109.540(10)
_cell_formula_units_Z            1
_cell_length_a                   6.4930(10)
_cell_length_b                   9.4880(20)
_cell_length_c                   10.5770(20)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      20.00
_cell_volume                     581.0(2)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_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           'Copper K\a    '
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1898
_diffrn_reflns_theta_max         59.85
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.12
_exptl_absorpt_correction_T_max  0.2159
_exptl_absorpt_correction_T_min  0.0611
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_F_000             350.02
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.35
_refine_diff_density_max         3.47
_refine_diff_density_min         -2.45
_refine_ls_extinction_coef       27198(1597)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   1.89
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1724
_refine_ls_R_factor_all          0.045
_refine_ls_R_factor_obs          0.045
_refine_ls_shift/esd_max         0.025
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(\s^2^(F)+0.0010F^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.060
_refine_ls_wR_factor_obs         0.060
_reflns_number_observed          1724
_reflns_number_total             1724
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            ic9510167_2.cif
_cod_data_source_block           C12H32O10P4Cl2Re
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+0.0010F^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)+0.0010F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        581.00(19)
_cod_original_formula_sum        'C12 H32 O10 P4 Cl2 Re '
_cod_database_code               4324060