Re Tricarbonyl Complexes with Ligands Containing P,N,N and P,N,O Donor Atom Sets: Synthesis and Structural Characterization
João D. G. Correia; Ângela Domingos; Isabel Santos; Roger Alberto; Kirstin Ortner; Inorganic Chemistry 40 (2001) 5147–5151; doi:10.1021/ic010417l

data_4320314
_publ_contact_author_address
;  'Departamento de Quimica, ITN, Estrada Nacional 10,
     2686-953 Sacavem, Codex, Portugal'
;
_publ_contact_author_email       isantos@itn1.itn.pt
_publ_contact_author_fax         '00351-219 94 14 55'
_publ_contact_author_name        'Isabel Santos'
_publ_contact_author_phone       '00351-219 94 62 01'
_publ_section_title
;
 Re Tricarbonyl Complexes with Ligands Containing P,N,N and P,N,O Donor
 Atom Sets: Synthesis and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5147
_journal_page_last               5151
_journal_paper_doi               10.1021/ic010417l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '[Re(CO)3Br(k2-H2PNO)]'
_chemical_formula_sum            'C24 H20 Br N O5 P Re'
_chemical_formula_weight         699.49
_chemical_name_common            '[Re(CO)3Br(k2-H2PNO)]'
_chemical_name_systematic        Rhenium(I)-(k2H2PNO)tricarbonylbromide
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.883(11)
_cell_angle_beta                 71.163(10)
_cell_angle_gamma                63.650(9)
_cell_formula_units_Z            2
_cell_length_a                   10.0241(9)
_cell_length_b                   11.2060(10)
_cell_length_c                   13.0656(12)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    183(2)
_cell_volume                     1242.2(2)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_molecular_graphics    'Zortep (Zsolnai, 1994), Platon (Spek, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f oscillation 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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10153
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  7.3
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    6.598
_exptl_absorpt_correction_T_max  0.7338
_exptl_absorpt_correction_T_min  0.5583
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                3493
_reflns_number_total             4500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010417l_2.cif
_cod_data_source_block           jg110500
_cod_original_cell_volume        1242.19(19)
_cod_database_code               4320314