#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:41:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179342 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/39/4323939.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_4323939
loop_
_publ_author_name
'Cristina Bolzati'
'Francesco Tisato'
'Fiorenzo Refosco'
'Giuliano Bandoli'
'Alessandro Dolmella'
_publ_section_title
;
 Uncommon Anionic Dioxorhenium(V) and Neutral Monooxorhenium(V)
 Mixed-Ligand Complexes Containing Heterofunctionalized Phosphine Ligands:
 Syntheses and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6221
_journal_page_last               6229
_journal_paper_doi               10.1021/ic960404l
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C34 H50 Cl3 N O2 P Re'
_chemical_formula_weight         828.27
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.91(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.840(3)
_cell_length_b                   22.167(6)
_cell_length_c                   15.210(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      9
_cell_volume                     3635.4(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet R3m/V automated diffractometer '
_diffrn_measurement_method       'omega-2 theta'
_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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6101
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.637
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            emerald_green
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.895
_refine_ls_goodness_of_fit_obs   0.994
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.619
_refine_ls_restrained_S_obs      0.994
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_obs          0.0505
_refine_ls_shift/esd_max         -0.232
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2480
_refine_ls_wR_factor_obs         0.1295
_reflns_number_observed          4134
_reflns_number_total             5832
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960404l_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323939
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.24970(3) 0.15365(2) 0.68218(2) 0.0580(2) Uani 1 d . .
Cl1 Cl 0.2036(3) 0.25379(13) 0.7287(3) 0.1151(13) Uani 1 d . .
Cl2 Cl 0.3353(2) 0.06215(13) 0.6347(2) 0.0784(7) Uani 1 d . .
Cl3 Cl 0.3263(2) 0.1979(2) 0.5568(2) 0.1029(12) Uani 1 d . .
P1 P 0.2242(2) 0.11206(9) 0.82645(13) 0.0414(5) Uani 1 d . .
O1 O 0.1015(6) 0.1362(4) 0.6522(4) 0.088(2) Uani 1 d . .
O2 O 0.4140(5) 0.1698(3) 0.7530(5) 0.067(2) Uani 1 d . .
C1 C 0.3488(7) 0.1475(3) 0.8923(6) 0.049(2) Uani 1 d . .
C2 C 0.3639(9) 0.1518(4) 0.9839(6) 0.061(2) Uani 1 d . .
C3 C 0.4673(9) 0.1826(5) 1.0241(8) 0.078(3) Uani 1 d . .
C4 C 0.5507(8) 0.2078(5) 0.9729(10) 0.091(4) Uani 1 d . .
C5 C 0.5354(8) 0.2028(5) 0.8805(8) 0.082(3) Uani 1 d . .
C6 C 0.4341(8) 0.1744(4) 0.8396(7) 0.062(2) Uani 1 d . .
C1A C 0.2468(6) 0.0321(4) 0.8380(5) 0.045(2) Uani 1 d . .
C2A C 0.1677(8) -0.0069(4) 0.7860(6) 0.066(2) Uani 1 d . .
C3A C 0.1841(10) -0.0680(5) 0.7910(6) 0.072(3) Uani 1 d . .
C4A C 0.2793(11) -0.0916(4) 0.8461(7) 0.075(3) Uani 1 d . .
C5A C 0.3569(10) -0.0546(4) 0.8970(7) 0.072(3) Uani 1 d . .
C6A C 0.3412(7) 0.0061(4) 0.8930(6) 0.056(2) Uani 1 d . .
C1B C 0.0842(7) 0.1255(4) 0.8798(5) 0.046(2) Uani 1 d . .
C2B C 0.0143(8) 0.1764(4) 0.8598(6) 0.059(2) Uani 1 d . .
C3B C -0.0872(8) 0.1885(5) 0.9075(7) 0.071(3) Uani 1 d . .
C4B C -0.1204(9) 0.1492(4) 0.9688(7) 0.070(3) Uani 1 d . .
C5B C -0.0508(8) 0.0986(5) 0.9889(6) 0.069(3) Uani 1 d . .
C6B C 0.0499(7) 0.0867(4) 0.9444(6) 0.058(2) Uani 1 d . .
N1 N 0.7284(6) 0.1337(3) 0.5666(5) 0.064(2) Uani 1 d . .
C1C C 0.8380(10) 0.1517(5) 0.5163(7) 0.082(3) Uiso 1 d . .
C2C C 0.9078(9) 0.1020(5) 0.4788(7) 0.080(3) Uiso 1 d . .
C3C C 1.0166(10) 0.1237(5) 0.4304(8) 0.090(3) Uiso 1 d . .
C4C C 1.1002(11) 0.0752(6) 0.4054(8) 0.098(4) Uiso 1 d . .
C1D C 0.6352(11) 0.0964(6) 0.5076(8) 0.098(4) Uiso 1 d . .
C2D C 0.5912(14) 0.1214(7) 0.4200(10) 0.124(5) Uiso 1 d . .
C3D C 0.4818(13) 0.0863(7) 0.3735(9) 0.129(5) Uiso 1 d . .
C4D C 0.4375(18) 0.1160(9) 0.2919(14) 0.172(7) Uiso 1 d . .
C1E C 0.6613(11) 0.1900(6) 0.5906(9) 0.103(4) Uiso 1 d . .
C2E C 0.7272(13) 0.2299(7) 0.6539(10) 0.123(5) Uiso 1 d . .
C3E C 0.6371(25) 0.2901(14) 0.6512(19) 0.222(12) Uiso 1 d . .
C4E C 0.6497(33) 0.3219(16) 0.6991(25) 0.270(16) Uiso 1 d . .
C1F C 0.7784(10) 0.0982(5) 0.6445(7) 0.083(3) Uiso 1 d . .
C2F C 0.6911(10) 0.0822(6) 0.7104(7) 0.089(3) Uiso 1 d . .
C3F C 0.7535(11) 0.0433(6) 0.7856(8) 0.098(4) Uiso 1 d . .
C4F C 0.6679(13) 0.0285(7) 0.8542(9) 0.116(4) Uiso 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'
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'
Cl Cl 0.1484 0.1585 '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
O1 Re O2 163.6(3) . . yes
O1 Re Cl3 106.4(2) . . yes
O2 Re Cl3 89.6(2) . . yes
O1 Re Cl2 96.6(3) . . yes
O2 Re Cl2 87.9(2) . . yes
Cl3 Re Cl2 85.88(10) . . yes
O1 Re Cl1 94.1(3) . . yes
O2 Re Cl1 82.9(2) . . yes
Cl3 Re Cl1 87.44(12) . . yes
Cl2 Re Cl1 168.70(10) . . yes
O1 Re P1 87.9(2) . . yes
O2 Re P1 76.1(2) . . yes
Cl3 Re P1 165.66(8) . . yes
Cl2 Re P1 92.02(8) . . yes
Cl1 Re P1 92.20(9) . . yes
C1 P1 C1A 107.0(3) . . ?
C1 P1 C1B 107.2(4) . . ?
C1A P1 C1B 103.3(3) . . ?
C1 P1 Re 101.0(3) . . yes
C1A P1 Re 115.9(2) . . ?
C1B P1 Re 121.3(3) . . ?
C6 O2 Re 126.5(5) . . yes
C2 C1 C6 121.5(8) . . ?
C2 C1 P1 126.8(7) . . ?
C6 C1 P1 111.7(7) . . ?
C3 C2 C1 118.6(10) . . ?
C2 C3 C4 119.7(10) . . ?
C5 C4 C3 121.4(9) . . ?
C4 C5 C6 120.1(10) . . ?
O2 C6 C5 122.4(10) . . ?
O2 C6 C1 118.8(8) . . ?
C5 C6 C1 118.7(10) . . ?
C2A C1A C6A 117.1(8) . . ?
C2A C1A P1 118.9(6) . . ?
C6A C1A P1 123.9(6) . . ?
C1A C2A C3A 120.7(9) . . ?
C4A C3A C2A 120.0(9) . . ?
C3A C4A C5A 120.3(9) . . ?
C6A C5A C4A 120.3(10) . . ?
C5A C6A C1A 121.6(9) . . ?
C2B C1B C6B 119.0(7) . . ?
C2B C1B P1 120.2(6) . . ?
C6B C1B P1 120.8(6) . . ?
C1B C2B C3B 119.1(8) . . ?
C4B C3B C2B 120.7(9) . . ?
C3B C4B C5B 120.2(9) . . ?
C4B C5B C6B 119.9(9) . . ?
C1B C6B C5B 121.1(8) . . ?
C1F N1 C1E 113.1(8) . . ?
C1F N1 C1D 110.4(8) . . ?
C1E N1 C1D 106.5(8) . . ?
C1F N1 C1C 107.5(7) . . ?
C1E N1 C1C 108.9(8) . . ?
C1D N1 C1C 110.4(8) . . ?
C2C C1C N1 116.8(8) . . ?
C1C C2C C3C 113.6(9) . . ?
C4C C3C C2C 114.7(10) . . ?
C2D C1D N1 117.5(11) . . ?
C1D C2D C3D 112.9(13) . . ?
C4D C3D C2D 109.8(15) . . ?
C2E C1E N1 116.8(11) . . ?
C1E C2E C3E 103.2(14) . . ?
C4E C3E C2E 120.6(36) . . ?
N1 C1F C2F 117.4(9) . . ?
C1F C2F C3F 111.9(10) . . ?
C4F C3F C2F 112.5(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
Re O1 1.669(6) . yes
Re O2 2.016(6) . yes
Re Cl3 2.369(2) . yes
Re Cl2 2.374(3) . yes
Re Cl1 2.398(3) . yes
Re P1 2.422(2) . yes
P1 C1 1.780(8) . yes
P1 C1A 1.794(8) . yes
P1 C1B 1.818(8) . yes
O2 C6 1.317(11) . yes
C1 C2 1.388(13) . ?
C1 C6 1.417(12) . ?
C2 C3 1.399(13) . ?
C3 C4 1.37(2) . ?
C4 C5 1.40(2) . ?
C5 C6 1.359(12) . ?
C1A C2A 1.404(11) . ?
C1A C6A 1.380(10) . ?
C2A C3A 1.367(13) . ?
C3A C4A 1.365(14) . ?
C4A C5A 1.357(13) . ?
C5A C6A 1.357(12) . ?
C1B C2B 1.375(11) . ?
C1B C6B 1.387(11) . ?
C2B C3B 1.405(12) . ?
C3B C4B 1.353(13) . ?
C4B C5B 1.368(13) . ?
C5B C6B 1.368(11) . ?
N1 C1F 1.479(12) . ?
N1 C1E 1.507(14) . ?
N1 C1D 1.524(13) . ?
N1 C1C 1.530(12) . ?
C1C C2C 1.484(13) . ?
C2C C3C 1.531(14) . ?
C3C C4C 1.48(2) . ?
C1D C2D 1.48(2) . ?
C2D C3D 1.53(2) . ?
C3D C4D 1.44(2) . ?
C1E C2E 1.44(2) . ?
C2E C3E 1.65(3) . ?
C3E C4E 1.01(4) . ?
C1F C2F 1.490(14) . ?
C2F C3F 1.534(15) . ?
C3F C4F 1.50(2) . ?
