#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:52:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179214 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314244.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4314244
loop_
_publ_author_name
'Torsten Kniess'
'João D. G. Correia'
'Ângela Domingos'
'Elisa Palma'
'Isabel Santos'
_publ_section_title
;
 Synthesis and Structural Characterization of Novel Re(I) Tricarbonyl
 Complexes Anchored on a Phosphinoarylbenzylamine and a
 Phosphinoaryloxazoline Generated in Situ
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6130
_journal_page_last               6135
_journal_paper_doi               10.1021/ic034372v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C24 H22 Br N O4 P Re'
_chemical_formula_sum            'C24 H22 Br N O4 P Re'
_chemical_formula_weight         685.51
_chemical_name_systematic
;
 ?
;
_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                 105.742(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2777(10)
_cell_length_b                   10.3652(8)
_cell_length_c                   20.7153(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      8.1
_cell_volume                     2330.7(3)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MolEN(Fair,1990)
_computing_molecular_graphics    ORTEP-3(Farrugia,1997)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick,1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       ω/2\qscans
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5866
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.028
_exptl_absorpt_correction_T_max  0.9993
_exptl_absorpt_correction_T_min  0.2972
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.152
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.00018(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+17.8482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                4218
_reflns_number_total             5590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034372vsi20030407_013301_1.cif
_cod_data_source_block           ks376
_cod_database_code               4314244
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.26896(2) 0.14582(3) 0.805985(14) 0.02303(10) Uani 1 1 d . . .
Br1 Br 0.41513(8) -0.05603(9) 0.83089(5) 0.0394(2) Uani 1 1 d . . .
P1 P 0.15153(16) 0.07453(19) 0.88411(9) 0.0232(4) Uani 1 1 d . . .
N1 N 0.4143(6) 0.2259(6) 0.8957(3) 0.0286(14) Uani 1 1 d . . .
H1 H 0.4867 0.1977 0.8893 0.034 Uiso 1 1 calc R . .
O2 O 0.1307(6) 0.3998(6) 0.7842(4) 0.0508(17) Uani 1 1 d . . .
O1 O 0.4196(6) 0.2129(7) 0.7066(3) 0.0470(16) Uani 1 1 d . . .
C111 C -0.0784(8) 0.1719(8) 0.8132(5) 0.041(2) Uani 1 1 d . . .
H111 H -0.0338 0.2351 0.7981 0.049 Uiso 1 1 calc R . .
C6 C 0.4122(7) 0.1674(8) 0.9618(4) 0.0319(17) Uani 1 1 d . . .
H6A H 0.4895 0.1857 0.9948 0.038 Uiso 1 1 calc R . .
H6B H 0.4044 0.0744 0.9569 0.038 Uiso 1 1 calc R . .
C2 C 0.1805(7) 0.3031(9) 0.7920(4) 0.0352(18) Uani 1 1 d . . .
C11 C -0.0167(6) 0.0742(8) 0.8547(4) 0.0277(16) Uani 1 1 d . . .
C105 C 0.0902(8) 0.2362(8) 0.9793(4) 0.0334(17) Uani 1 1 d . . .
H105 H 0.0090 0.2112 0.9604 0.040 Uiso 1 1 calc R . .
C101 C 0.3070(7) 0.2188(7) 0.9868(4) 0.0273(15) Uani 1 1 d . . .
C115 C -0.0866(7) -0.0213(8) 0.8748(4) 0.0336(18) Uani 1 1 d . . .
H115 H -0.0470 -0.0888 0.9017 0.040 Uiso 1 1 calc R . .
C10 C 0.1837(7) 0.1835(7) 0.9557(4) 0.0273(16) Uani 1 1 d . . .
C12 C 0.1858(6) -0.0865(8) 0.9185(4) 0.0277(16) Uani 1 1 d . . .
C4 C 0.4301(8) 0.3683(8) 0.9020(5) 0.0396(19) Uani 1 1 d . . .
H4A H 0.4934 0.3873 0.9430 0.047 Uiso 1 1 calc R . .
H4B H 0.3537 0.4062 0.9059 0.047 Uiso 1 1 calc R . .
C102 C 0.3327(8) 0.3032(9) 1.0405(4) 0.040(2) Uani 1 1 d . . .
H102 H 0.4141 0.3232 1.0623 0.048 Uiso 1 1 calc R . .
C103 C 0.2380(9) 0.3584(10) 1.0622(4) 0.045(2) Uani 1 1 d . . .
H103 H 0.2560 0.4171 1.0975 0.054 Uiso 1 1 calc R . .
C1 C 0.3662(7) 0.1920(8) 0.7451(4) 0.0347(18) Uani 1 1 d . . .
C5 C 0.4649(8) 0.4310(9) 0.8439(4) 0.041(2) Uani 1 1 d . . .
H5A H 0.3998 0.4182 0.8028 0.049 Uiso 1 1 calc R . .
H5B H 0.4764 0.5230 0.8517 0.049 Uiso 1 1 calc R . .
O4 O 0.5750(6) 0.3747(7) 0.8378(3) 0.0547(19) Uani 1 1 d . . .
H4 H 0.5943 0.4073 0.8060 0.082 Uiso 1 1 calc R . .
C125 C 0.2235(7) -0.1113(9) 0.9861(4) 0.0364(19) Uani 1 1 d . . .
H125 H 0.2359 -0.0436 1.0166 0.044 Uiso 1 1 calc R . .
C113 C -0.2729(8) 0.0838(10) 0.8148(5) 0.045(2) Uani 1 1 d . . .
H113 H -0.3585 0.0880 0.8019 0.054 Uiso 1 1 calc R . .
C121 C 0.1687(8) -0.1887(8) 0.8732(5) 0.040(2) Uani 1 1 d . . .
H121 H 0.1443 -0.1721 0.8274 0.047 Uiso 1 1 calc R . .
C124 C 0.2435(8) -0.2400(10) 1.0091(5) 0.049(2) Uani 1 1 d . . .
H124 H 0.2681 -0.2576 1.0548 0.059 Uiso 1 1 calc R . .
C112 C -0.2051(8) 0.1759(10) 0.7942(5) 0.048(2) Uani 1 1 d . . .
H112 H -0.2451 0.2427 0.7668 0.058 Uiso 1 1 calc R . .
C114 C -0.2130(8) -0.0167(10) 0.8555(5) 0.044(2) Uani 1 1 d . . .
H114 H -0.2585 -0.0804 0.8695 0.053 Uiso 1 1 calc R . .
C123 C 0.2265(10) -0.3380(10) 0.9637(6) 0.056(3) Uani 1 1 d . . .
H123 H 0.2414 -0.4225 0.9789 0.068 Uiso 1 1 calc R . .
C3 C 0.1530(8) 0.0677(9) 0.7303(4) 0.0363(19) Uani 1 1 d . . .
C104 C 0.1171(9) 0.3260(8) 1.0312(4) 0.039(2) Uani 1 1 d . . .
H104 H 0.0536 0.3643 1.0451 0.047 Uiso 1 1 calc R . .
C122 C 0.1877(10) -0.3144(9) 0.8956(6) 0.053(3) Uani 1 1 d . . .
H122 H 0.1745 -0.3824 0.8651 0.064 Uiso 1 1 calc R . .
O3 O 0.0871(7) 0.0216(9) 0.6848(4) 0.066(2) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Re1 C3 91.4(4) . . ?
C2 Re1 C1 93.2(4) . . ?
C3 Re1 C1 87.3(3) . . ?
C2 Re1 N1 92.5(3) . . ?
C3 Re1 N1 176.0(3) . . ?
C1 Re1 N1 91.8(3) . . ?
C2 Re1 P1 90.2(3) . . ?
C3 Re1 P1 92.4(2) . . ?
C1 Re1 P1 176.6(3) . . ?
N1 Re1 P1 88.27(16) . . ?
C2 Re1 Br1 173.3(3) . . ?
C3 Re1 Br1 94.4(3) . . ?
C1 Re1 Br1 83.6(3) . . ?
N1 Re1 Br1 81.68(17) . . ?
P1 Re1 Br1 93.01(5) . . ?
C12 P1 C10 106.1(4) . . ?
C12 P1 C11 102.7(3) . . ?
C10 P1 C11 103.4(3) . . ?
C12 P1 Re1 116.0(2) . . ?
C10 P1 Re1 109.0(2) . . ?
C11 P1 Re1 118.4(3) . . ?
C4 N1 C6 110.5(6) . . ?
C4 N1 Re1 118.5(5) . . ?
C6 N1 Re1 114.2(4) . . ?
C112 C111 C11 120.4(8) . . ?
N1 C6 C101 112.2(6) . . ?
O2 C2 Re1 177.8(8) . . ?
C111 C11 C115 118.2(7) . . ?
C111 C11 P1 120.4(6) . . ?
C115 C11 P1 121.4(6) . . ?
C10 C105 C104 120.5(8) . . ?
C102 C101 C10 119.8(7) . . ?
C102 C101 C6 119.1(7) . . ?
C10 C101 C6 121.2(7) . . ?
C114 C115 C11 120.9(8) . . ?
C105 C10 C101 118.9(7) . . ?
C105 C10 P1 121.9(6) . . ?
C101 C10 P1 119.1(6) . . ?
C125 C12 C121 119.5(8) . . ?
C125 C12 P1 123.1(6) . . ?
C121 C12 P1 117.3(6) . . ?
N1 C4 C5 114.0(7) . . ?
C101 C102 C103 120.6(8) . . ?
C104 C103 C102 119.9(8) . . ?
O1 C1 Re1 175.5(8) . . ?
O4 C5 C4 108.6(7) . . ?
C12 C125 C124 119.8(9) . . ?
C112 C113 C114 119.5(8) . . ?
C122 C121 C12 120.7(9) . . ?
C123 C124 C125 119.5(9) . . ?
C113 C112 C111 121.1(9) . . ?
C115 C114 C113 119.8(8) . . ?
C124 C123 C122 121.3(9) . . ?
O3 C3 Re1 178.1(8) . . ?
C103 C104 C105 120.1(8) . . ?
C121 C122 C123 119.2(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C2 1.892(9) . ?
Re1 C3 1.927(9) . ?
Re1 C1 1.942(8) . ?
Re1 N1 2.275(6) . ?
Re1 P1 2.4661(18) . ?
Re1 Br1 2.6267(9) . ?
P1 C12 1.815(8) . ?
P1 C10 1.820(8) . ?
P1 C11 1.828(7) . ?
N1 C4 1.488(10) . ?
N1 C6 1.505(9) . ?
O2 C2 1.138(10) . ?
O1 C1 1.145(10) . ?
C111 C112 1.376(12) . ?
C111 C11 1.388(11) . ?
C6 C101 1.514(10) . ?
C11 C115 1.397(10) . ?
C105 C10 1.390(10) . ?
C105 C104 1.392(11) . ?
C101 C102 1.382(11) . ?
C101 C10 1.414(10) . ?
C115 C114 1.373(11) . ?
C12 C125 1.372(11) . ?
C12 C121 1.394(12) . ?
C4 C5 1.511(12) . ?
C102 C103 1.388(13) . ?
C103 C104 1.382(13) . ?
C5 O4 1.408(11) . ?
C125 C124 1.414(12) . ?
C113 C112 1.363(14) . ?
C113 C114 1.393(14) . ?
C121 C122 1.380(13) . ?
C124 C123 1.361(15) . ?
C123 C122 1.382(16) . ?
C3 O3 1.135(10) . ?
