Novel Coordination Behavior of fac-[ReBr3(CO)3]2- with 1,3,5-Triaza-7-phosphaadamantane (PTA). Systematic Investigation on Stepwise Replacement of the Halides by PTA Ligand. Phase Transfer Studies and X-ray Crystal Structure of [NEt4][ReBr2((PTA)(CO)3], [ReBr(PTA)2(CO)3], and [Re(PTA)3(CO)3]PF6
Roger Schibli; Kattesh V. Katti; Wynn A. Volkert; Charles L. Barnes; Inorganic Chemistry 37 (1998) 5306–5312; doi:10.1021/ic980373p

data_4323065
_publ_contact_author
;
Prof. Kattesh V. Katti
Center for Radiological Research
Business Loop 70 West
Allton Bldg. Room 106
Columbia, MO 65211
;
_publ_section_title
;
 Novel Coordination Behavior of fac-[ReBr3(CO)3]2- with
 1,3,5-Triaza-7-phosphaadamantane (PTA). Systematic Investigation on
 Stepwise Replacement of the Halides by PTA Ligand. Phase Transfer Studies
 and X-ray Crystal Structure of [NEt4][ReBr2((PTA)(CO)3],
 [ReBr(PTA)2(CO)3], and [Re(PTA)3(CO)3]PF6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5306
_journal_page_last               5312
_journal_paper_doi               10.1021/ic980373p
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C15 H24 N6 O3 P2 Br Re '
_chemical_formula_sum            'C15 H24 Br N6 O3 P2 Re'
_chemical_formula_weight         664.44
_chemical_name_common            '[ReBr(PTA)2(CO)3]'
_chemical_name_systematic
;
 [bromo tricarbonyl di(1,3,5-Triaza-7-Phosphaadamantane)rhenium(I)]
;
_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'
_cell_angle_alpha                90.0
_cell_angle_beta                 94.6650(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   6.8581(4)
_cell_length_b                   21.9499(12)
_cell_length_c                   13.9526(8)
_cell_measurement_reflns_used    6633
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      5.00
_cell_volume                     2093.4(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Siemens SMART CCD       '
_diffrn_measurement_method       'Omega scan b/P/b        '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12373
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    7.95
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_F_000             1274.92
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.30
_refine_diff_density_min         -0.97
_refine_ls_goodness_of_fit_obs   0.89
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3521
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_obs          0.036
_refine_ls_shift/esd_max         0.000
_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         0.042
_refine_ls_wR_factor_obs         0.042
_reflns_number_observed          3521
_reflns_number_total             4533
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            ic980373p_4.cif
_cod_data_source_block           ?
_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        2093.39(21)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C15 H24 N6 O3 P2 Br Re '
_cod_database_code               4323065