#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:23:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179325 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322220.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_4322220
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Marina A. Petrukhina'
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 6. Rare or
 Unprecedented Isomers of [Re2Cl6(PR3)2] Stoichiometry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3889
_journal_page_last               3894
_journal_paper_doi               10.1021/ic9906095
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 Re2 Cl4 ((C6 H5)2 P (C H2)3 P (C6 H5)2)2, 4 (C H2 Cl2)
;
_chemical_formula_structural     \a-Re2Cl4(dppp)2,4CH2Cl2
_chemical_formula_sum            'C58 H60 Cl12 P4 Re2'
_chemical_formula_weight         1678.74
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Tetrachloro-bis(1,3-bis(diphenylphosphino)-propane-
 -di-rhenium (II, II), dichloromethane solvate
;
_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
_cell_angle_alpha                83.41(1)
_cell_angle_beta                 74.80(2)
_cell_angle_gamma                63.02(2)
_cell_formula_units_Z            1
_cell_length_a                   11.830(3)
_cell_length_b                   12.134(2)
_cell_length_c                   12.356(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      18
_cell_volume                     1525.3(6)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V.5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9926
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.634
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.7475
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.45
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_obs          0.0231
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0268P)²+2.3289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0605
_refine_ls_wR_factor_obs         0.0599
_reflns_number_observed          6413
_reflns_number_total             6623
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9906095_1.cif
_cod_data_source_block           alpha-Re2Cl4(dppp)2,4CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+2.3289P] 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^)+(0.0268P)^2^+2.3289P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1525.3(5)
_cod_database_code               4322220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Re1 Re 0.415964(10) 0.074463(9) 0.057565(9) 0.01312(5) Uani 1 d . .
Cl1 Cl 0.21333(7) 0.11670(7) 0.01500(6) 0.02132(15) Uani 1 d . .
Cl2 Cl 0.37049(7) 0.27522(6) -0.02243(6) 0.01948(14) Uani 1 d . .
P1 P 0.53306(8) 0.11610(7) 0.16700(6) 0.01614(15) Uani 1 d . .
P2 P 0.36606(8) -0.05109(7) 0.21108(7) 0.0171(2) Uani 1 d . .
C1 C 0.6442(3) 0.1885(3) 0.1157(3) 0.0211(6) Uani 1 d . .
C2 C 0.5912(4) 0.3145(3) 0.0893(3) 0.0247(7) Uani 1 d . .
H2 H 0.5018(4) 0.3578(3) 0.0872(3) 0.030 Uiso 1 calc R .
C3 C 0.6689(4) 0.3765(4) 0.0662(3) 0.0319(8) Uani 1 d . .
H3 H 0.6325(4) 0.4618(4) 0.0478(3) 0.038 Uiso 1 calc R .
C4 C 0.7979(4) 0.3151(4) 0.0699(3) 0.0359(9) Uani 1 d . .
H4 H 0.8497(4) 0.3586(4) 0.0564(3) 0.043 Uiso 1 calc R .
C5 C 0.8527(4) 0.1897(4) 0.0933(3) 0.0372(9) Uani 1 d . .
H5 H 0.9425(4) 0.1472(4) 0.0941(3) 0.045 Uiso 1 calc R .
C6 C 0.7767(4) 0.1260(4) 0.1156(3) 0.0293(7) Uani 1 d . .
H6 H 0.8149(4) 0.0399(4) 0.1309(3) 0.035 Uiso 1 calc R .
C7 C 0.4139(3) 0.2297(3) 0.2761(3) 0.0180(6) Uani 1 d . .
C8 C 0.4498(4) 0.2394(3) 0.3731(3) 0.0264(7) Uani 1 d . .
H8 H 0.5350(4) 0.1856(3) 0.3826(3) 0.032 Uiso 1 calc R .
C9 C 0.3626(4) 0.3266(3) 0.4546(3) 0.0294(8) Uani 1 d . .
H9 H 0.3885(4) 0.3322(3) 0.5196(3) 0.035 Uiso 1 calc R .
C10 C 0.2383(4) 0.4056(3) 0.4428(3) 0.0279(7) Uani 1 d . .
H10 H 0.1790(4) 0.4655(3) 0.4991(3) 0.033 Uiso 1 calc R .
C11 C 0.2009(4) 0.3969(3) 0.3490(3) 0.0295(8) Uani 1 d . .
H11 H 0.1148(4) 0.4498(3) 0.3412(3) 0.035 Uiso 1 calc R .
C12 C 0.2890(3) 0.3106(3) 0.2654(3) 0.0245(7) Uani 1 d . .
H12 H 0.2629(3) 0.3073(3) 0.1998(3) 0.029 Uiso 1 calc R .
C13 C 0.6244(3) -0.0118(3) 0.2508(3) 0.0210(6) Uani 1 d . .
H13A H 0.6933(3) -0.0794(3) 0.1995(3) 0.025 Uiso 1 calc R .
H13B H 0.6683(3) 0.0169(3) 0.2912(3) 0.025 Uiso 1 calc R .
C14 C 0.5418(3) -0.0637(3) 0.3361(3) 0.0215(6) Uani 1 d . .
H14A H 0.5932(3) -0.1157(3) 0.3900(3) 0.026 Uiso 1 calc R .
H14B H 0.4641(3) 0.0060(3) 0.3786(3) 0.026 Uiso 1 calc R .
C15 C 0.4965(3) -0.1404(3) 0.2849(3) 0.0200(6) Uani 1 d . .
H15A H 0.4653(3) -0.1881(3) 0.3454(3) 0.024 Uiso 1 calc R .
H15B H 0.5725(3) -0.2006(3) 0.2315(3) 0.024 Uiso 1 calc R .
C16 C 0.2302(3) 0.0471(3) 0.3234(3) 0.0226(7) Uani 1 d . .
C17 C 0.1266(4) 0.1541(3) 0.2996(3) 0.0294(8) Uani 1 d . .
H17 H 0.1289(4) 0.1812(3) 0.2242(3) 0.035 Uiso 1 calc R .
C18 C 0.0197(4) 0.2224(4) 0.3843(4) 0.0403(10) Uani 1 d . .
H18 H -0.0492(4) 0.2962(4) 0.3665(4) 0.048 Uiso 1 calc R .
C19 C 0.0134(4) 0.1839(4) 0.4928(4) 0.0447(10) Uani 1 d . .
H19 H -0.0605(4) 0.2298(4) 0.5503(4) 0.054 Uiso 1 calc R .
C20 C 0.1154(5) 0.0771(5) 0.5188(4) 0.0514(12) Uani 1 d . .
H20 H 0.1120(5) 0.0506(5) 0.5945(4) 0.062 Uiso 1 calc R .
C21 C 0.2221(4) 0.0091(4) 0.4346(3) 0.0378(9) Uani 1 d . .
H21 H 0.2908(4) -0.0645(4) 0.4531(3) 0.045 Uiso 1 calc R .
C22 C 0.3049(3) -0.1634(3) 0.2008(3) 0.0204(6) Uani 1 d . .
C23 C 0.3760(3) -0.2894(3) 0.2169(3) 0.0231(7) Uani 1 d . .
H23 H 0.4634(3) -0.3210(3) 0.2237(3) 0.028 Uiso 1 calc R .
C24 C 0.3194(4) -0.3690(3) 0.2230(3) 0.0287(7) Uani 1 d . .
H24 H 0.3681(4) -0.4548(3) 0.2349(3) 0.034 Uiso 1 calc R .
C25 C 0.1928(4) -0.3244(3) 0.2120(3) 0.0295(8) Uani 1 d . .
H25 H 0.1544(4) -0.3791(3) 0.2170(3) 0.035 Uiso 1 calc R .
C26 C 0.1222(4) -0.1994(4) 0.1936(3) 0.0301(8) Uani 1 d . .
H26 H 0.0357(4) -0.1688(4) 0.1846(3) 0.036 Uiso 1 calc R .
C27 C 0.1772(4) -0.1189(3) 0.1883(3) 0.0274(7) Uani 1 d . .
H27 H 0.1281(4) -0.0332(3) 0.1761(3) 0.033 Uiso 1 calc R .
Cl3 Cl 0.86777(9) 0.67684(9) 0.27791(8) 0.0352(2) Uani 1 d . .
Cl4 Cl 1.02714(11) 0.46027(10) 0.13341(9) 0.0498(3) Uani 1 d . .
C28 C 0.9149(4) 0.6168(4) 0.1414(3) 0.0380(9) Uani 1 d . .
H28A H 0.8366(4) 0.6266(4) 0.1187(3) 0.046 Uiso 1 calc R .
H28B H 0.9545(4) 0.6645(4) 0.0884(3) 0.046 Uiso 1 calc R .
Cl5 Cl 0.69871(10) 0.49854(9) 0.30552(8) 0.0366(2) Uani 1 d . .
Cl6 Cl 0.65599(11) 0.34005(11) 0.49000(9) 0.0458(2) Uani 1 d . .
C29 C 0.6370(5) 0.3910(5) 0.3530(4) 0.0450(11) Uani 1 d . .
H29A H 0.6832(5) 0.3191(5) 0.3013(4) 0.054 Uiso 1 calc R .
H29B H 0.5432(5) 0.4290(5) 0.3529(4) 0.054 Uiso 1 calc R .
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'
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
Re1 Re1 Cl2 110.98(3) 2_655 . y
Re1 Re1 Cl1 110.20(3) 2_655 . y
Cl2 Re1 Cl1 82.27(3) . . y
Re1 Re1 P1 99.95(3) 2_655 . y
Cl2 Re1 P1 86.74(3) . . y
Cl1 Re1 P1 149.85(3) . . y
Re1 Re1 P2 99.99(3) 2_655 . y
Cl2 Re1 P2 149.03(3) . . y
Cl1 Re1 P2 87.54(3) . . y
P1 Re1 P2 87.65(3) . . y
C13 P1 C7 101.60(15) . . n
C13 P1 C1 102.00(15) . . n
C7 P1 C1 98.55(14) . . n
C13 P1 Re1 116.54(11) . . n
C7 P1 Re1 108.38(11) . . n
C1 P1 Re1 125.95(10) . . n
C22 P2 C15 102.03(15) . . n
C22 P2 C16 98.13(15) . . n
C15 P2 C16 102.8(2) . . n
C22 P2 Re1 124.46(10) . . n
C15 P2 Re1 115.70(11) . . n
C16 P2 Re1 110.51(11) . . n
C6 C1 C2 118.9(3) . . n
C6 C1 P1 121.9(3) . . n
C2 C1 P1 118.6(3) . . n
C3 C2 C1 120.2(3) . . n
C4 C3 C2 120.4(4) . . n
C3 C4 C5 120.2(3) . . n
C4 C5 C6 120.2(4) . . n
C5 C6 C1 120.0(4) . . n
C12 C7 C8 117.7(3) . . n
C12 C7 P1 122.4(2) . . n
C8 C7 P1 119.8(2) . . n
C9 C8 C7 120.6(3) . . n
C10 C9 C8 120.7(3) . . n
C11 C10 C9 119.5(3) . . n
C10 C11 C12 120.1(3) . . n
C7 C12 C11 121.2(3) . . n
C14 C13 P1 114.6(2) . . n
C15 C14 C13 114.3(3) . . n
C14 C15 P2 115.0(2) . . n
C17 C16 C21 117.7(3) . . n
C17 C16 P2 121.6(3) . . n
C21 C16 P2 120.4(3) . . n
C16 C17 C18 121.2(3) . . n
C19 C18 C17 120.3(4) . . n
C18 C19 C20 119.7(4) . . n
C21 C20 C19 120.1(4) . . n
C20 C21 C16 121.0(4) . . n
C23 C22 C27 119.1(3) . . n
C23 C22 P2 122.0(3) . . n
C27 C22 P2 118.5(3) . . n
C24 C23 C22 120.2(3) . . n
C25 C24 C23 120.5(3) . . n
C24 C25 C26 119.8(3) . . n
C25 C26 C27 120.3(3) . . n
C26 C27 C22 120.2(3) . . n
Cl4 C28 Cl3 111.8(2) . . n
Cl5 C29 Cl6 111.3(2) . . n
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 Re1 2.2559(8) 2_655 y
Re1 Cl2 2.3952(8) . y
Re1 Cl1 2.4021(10) . y
Re1 P1 2.4035(9) . y
Re1 P2 2.4151(9) . y
P1 C13 1.829(3) . n
P1 C7 1.836(3) . n
P1 C1 1.840(3) . n
P2 C22 1.839(3) . n
P2 C15 1.839(3) . n
P2 C16 1.844(3) . n
C1 C6 1.397(5) . n
C1 C2 1.400(5) . n
C2 C3 1.390(5) . n
C3 C4 1.372(6) . n
C4 C5 1.385(6) . n
C5 C6 1.391(5) . n
C7 C12 1.387(5) . n
C7 C8 1.405(4) . n
C8 C9 1.381(5) . n
C9 C10 1.379(5) . n
C10 C11 1.375(5) . n
C11 C12 1.394(5) . n
C13 C14 1.526(5) . n
C14 C15 1.523(4) . n
C16 C17 1.390(5) . n
C16 C21 1.391(5) . n
C17 C18 1.391(5) . n
C18 C19 1.362(6) . n
C19 C20 1.388(7) . n
C20 C21 1.386(6) . n
C22 C23 1.391(5) . n
C22 C27 1.400(5) . n
C23 C24 1.390(5) . n
C24 C25 1.381(5) . n
C25 C26 1.386(5) . n
C26 C27 1.387(5) . n
Cl3 C28 1.763(4) . n
Cl4 C28 1.751(4) . n
Cl5 C29 1.744(4) . n
Cl6 C29 1.770(4) . n
