#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319799.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_4319799
loop_
_publ_author_name
'Jitendra K. Bera'
'Phillip E. Fanwick'
'Richard A. Walton'
_publ_contact_author_address
;    Department of Chemistry
      Purdue University
      W. Lafayette
      IN 47907
      USA
;
_publ_contact_author_email       rawalton@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Richard A. Walton'
_publ_contact_author_phone       1(765)4945464
_publ_section_title
;
 Reaction of Re2(μ-O2CCH3)4Cl2 with Bis(dicyclohexylphosphino)methane
 (dcpm): Isolation of the Mixed-Valent Complex O3ReReCl(η2-dcpm)2
 Containing an Unsupported Re-Re Bond
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2914
_journal_page_last               2917
_journal_paper_doi               10.1021/ic0100471
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C51 H94 Cl3 O3 P4 Re2'
_chemical_formula_weight         1357.97
_chemical_name_systematic        ' ?'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             4-08-00
_audit_creation_method           from_MolEN_and_SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0179(4)
_cell_length_b                   22.8589(5)
_cell_length_c                   13.5102(7)
_cell_measurement_reflns_used    34524
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5564.4(3)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
     ORTEP (Johnson, 1976)
     Xtal_GX (Hall, 1995)
     PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    Direct_methods_(Shelxs97,_Sheldrick,_1997)
_diffrn_ambient_temperature      150
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34524
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    4.703
_exptl_absorpt_correction_T_max  0.3904
_exptl_absorpt_correction_T_min  0.3299
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_description       needle
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.38
_refine_diff_density_min         -1.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6464
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0467P)²+27.3572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.106
_reflns_number_gt                10031
_reflns_number_total             12622
_reflns_threshold_expression     >2.0σ(I)
_cod_data_source_file            ic0100471.cif
_cod_data_source_block           SDC25R
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5564.4(5)
_cod_original_sg_symbol_H-M      'p n m a'
_cod_database_code               4319799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x+1/2, y, -z+1/2'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_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_calc_flag
Re(1) 0.109662(18) 0.7500 0.03034(2) 0.01632(9) Uani ?
Re(2) 0.00738(3) 0.72955(2) 0.15498(3) 0.01870(10) Uani ?
Cl(1) 0.21003(12) 0.7500 -0.09671(16) 0.0266(6) Uani ?
Cl(91) 0.4990(2) 0.2500 0.0546(2) 0.0688(12) Uani ?
Cl(92) 0.3392(3) 0.2500 0.0309(5) 0.130(3) Uani ?
P(1) 0.18939(9) 0.68988(7) 0.13896(12) 0.0185(4) Uani ?
P(2) 0.04611(9) 0.68935(7) -0.09686(11) 0.0201(4) Uani ?
O(21) 0.0401(4) 0.7500 0.2704(4) 0.0273(17) Uani ?
O(22) -0.0117(5) 0.6553(4) 0.1536(6) 0.024(2) Uani ?
O(23) -0.0725(5) 0.7323(4) 0.1258(6) 0.030(3) Uani ?
C(1B) 0.2124(5) 0.7500 0.2247(6) 0.021(2) Uani ?
C(2B) 0.0371(5) 0.7500 -0.1849(7) 0.024(2) Uani ?
C(111) 0.2819(3) 0.6672(3) 0.0922(4) 0.0210(15) Uani ?
C(112) 0.3381(4) 0.6465(3) 0.1685(5) 0.0263(17) Uani ?
C(113) 0.4158(4) 0.6435(4) 0.1213(5) 0.0353(18) Uani ?
C(114) 0.4168(4) 0.6040(3) 0.0299(5) 0.035(2) Uani ?
C(115) 0.3561(4) 0.6215(3) -0.0445(5) 0.032(2) Uani ?
C(116) 0.2802(4) 0.6238(3) 0.0046(5) 0.0247(15) Uani ?
C(121) 0.1489(4) 0.6323(3) 0.2188(5) 0.0263(15) Uani ?
C(122) 0.1253(4) 0.5784(3) 0.1597(5) 0.0317(18) Uani ?
C(123) 0.0746(4) 0.5394(3) 0.2227(6) 0.041(2) Uani ?
C(124) 0.1114(5) 0.5223(4) 0.3187(7) 0.054(3) Uani ?
C(125) 0.1393(5) 0.5750(5) 0.3751(6) 0.058(3) Uani ?
C(126) 0.1902(4) 0.6141(4) 0.3118(6) 0.043(2) Uani ?
C(211) 0.0957(4) 0.6337(3) -0.1728(5) 0.0243(17) Uani ?
C(212) 0.1168(3) 0.5766(3) -0.1215(5) 0.0247(15) Uani ?
C(213) 0.1724(4) 0.5432(3) -0.1849(5) 0.0320(18) Uani ?
C(214) 0.1401(4) 0.5299(3) -0.2867(6) 0.0363(18) Uani ?
C(215) 0.1126(5) 0.5848(4) -0.3377(5) 0.048(3) Uani ?
C(216) 0.0599(5) 0.6197(3) -0.2730(5) 0.040(2) Uani ?
C(221) -0.0503(4) 0.6643(3) -0.0731(5) 0.0273(17) Uani ?
C(222) -0.1005(6) 0.6594(9) -0.1617(7) 0.140(6) Uani ?
C(223) -0.1821(6) 0.6482(7) -0.1281(8) 0.098(5) Uani ?
C(224) -0.1839(7) 0.5940(5) -0.0681(14) 0.119(6) Uani ?
C(225) -0.1340(6) 0.5960(7) 0.0166(14) 0.130(7) Uani ?
C(226) -0.0531(5) 0.6092(5) -0.0135(12) 0.111(5) Uani ?
C(901) 0.4214(9) 0.2277(8) -0.0078(12) 0.053(5) Uani ?
H(111) 0.3035 0.7030 0.0646 0.0270 Uiso calc
H(11A) 0.3240 0.6081 0.1928 0.0340 Uiso calc
H(11B) 0.3388 0.6733 0.2241 0.0340 Uiso calc
H(11C) 0.4315 0.6825 0.1027 0.0460 Uiso calc
H(11D) 0.4509 0.6286 0.1697 0.0460 Uiso calc
H(11E) 0.4093 0.5638 0.0502 0.0450 Uiso calc
H(11F) 0.4650 0.6067 -0.0018 0.0450 Uiso calc
H(11G) 0.3677 0.6595 -0.0723 0.0410 Uiso calc
H(11H) 0.3550 0.5933 -0.0982 0.0410 Uiso calc
H(11I) 0.2668 0.5852 0.0283 0.0320 Uiso calc
H(11J) 0.2433 0.6361 -0.0432 0.0320 Uiso calc
H(121) 0.1023 0.6492 0.2429 0.0340 Uiso calc
H(12A) 0.1690 0.5565 0.1398 0.0410 Uiso calc
H(12B) 0.0992 0.5905 0.1004 0.0410 Uiso calc
H(12C) 0.0289 0.5601 0.2369 0.0530 Uiso calc
H(12D) 0.0622 0.5044 0.1857 0.0530 Uiso calc
H(12E) 0.1528 0.4964 0.3048 0.0700 Uiso calc
H(12F) 0.0762 0.5011 0.3595 0.0700 Uiso calc
H(12G) 0.1664 0.5618 0.4330 0.0750 Uiso calc
H(12H) 0.0972 0.5978 0.3976 0.0750 Uiso calc
H(12I) 0.2045 0.6485 0.3493 0.0560 Uiso calc
H(12J) 0.2349 0.5929 0.2942 0.0560 Uiso calc
H(1B1) 0.2644 0.7500 0.2436 0.0270 Uiso calc
H(1B2) 0.1814 0.7500 0.2833 0.0270 Uiso calc
H(211) 0.1433 0.6521 -0.1895 0.0320 Uiso calc
H(21A) 0.1384 0.5850 -0.0572 0.0320 Uiso calc
H(21B) 0.0727 0.5529 -0.1113 0.0320 Uiso calc
H(21C) 0.1855 0.5069 -0.1522 0.0420 Uiso calc
H(21D) 0.2172 0.5663 -0.1923 0.0420 Uiso calc
H(21E) 0.1779 0.5116 -0.3274 0.0470 Uiso calc
H(21F) 0.0993 0.5025 -0.2798 0.0470 Uiso calc
H(21G) 0.0874 0.5740 -0.3984 0.0630 Uiso calc
H(21H) 0.1548 0.6091 -0.3551 0.0630 Uiso calc
H(21I) 0.0147 0.5975 -0.2625 0.0510 Uiso calc
H(21J) 0.0469 0.6559 -0.3062 0.0510 Uiso calc
H(221) -0.0726 0.6944 -0.0311 0.0360 Uiso calc
H(22A) -0.0840 0.6275 -0.2036 0.1820 Uiso calc
H(22B) -0.0982 0.6953 -0.2000 0.1820 Uiso calc
H(22C) -0.1999 0.6809 -0.0891 0.1270 Uiso calc
H(22D) -0.2140 0.6439 -0.1855 0.1270 Uiso calc
H(22E) -0.2342 0.5876 -0.0447 0.1540 Uiso calc
H(22F) -0.1705 0.5611 -0.1098 0.1540 Uiso calc
H(22G) -0.1357 0.5587 0.0508 0.1700 Uiso calc
H(22H) -0.1509 0.6259 0.0622 0.1700 Uiso calc
H(22I) -0.0227 0.6135 0.0453 0.1440 Uiso calc
H(22J) -0.0335 0.5770 -0.0522 0.1440 Uiso calc
H(2B1) -0.0107 0.7500 -0.2179 0.0310 Uiso calc
H(2B2) 0.0765 0.7500 -0.2338 0.0310 Uiso calc
H(90A) 0.4267 0.2400 -0.0762 0.0690 Uiso calc
H(90B) 0.4210 0.1853 -0.0076 0.0690 Uiso calc
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
P(1) Re(1) P(1) 67.58(7) ?
P(1) Re(1) P(2) 171.10(5) ?
P(1) Re(1) P(2) 111.59(5) ?
P(1) Re(1) P(2) 111.59(5) ?
P(1) Re(1) P(2) 171.10(5) ?
P(2) Re(1) P(2) 67.76(7) ?
P(1) Re(1) Cl(1) 89.27(6) ?
P(1) Re(1) Cl(1) 89.27(6) ?
P(2) Re(1) Cl(1) 81.85(6) ?
P(2) Re(1) Cl(1) 81.85(6) ?
P(1) Re(1) Re(2) 85.74(4) ?
P(1) Re(1) Re(2) 97.49(4) ?
P(2) Re(1) Re(2) 103.10(4) ?
P(2) Re(1) Re(2) 91.23(4) ?
Cl(1) Re(1) Re(2) 169.337(12) ?
P(1) Re(1) Re(2) 97.49(4) ?
P(1) Re(1) Re(2) 85.74(4) ?
P(2) Re(1) Re(2) 91.23(4) ?
P(2) Re(1) Re(2) 103.10(4) ?
Cl(1) Re(1) Re(2) 169.338(12) ?
Re(2) Re(1) Re(2) 21.22(2) ?
Re(2) Re(2) O(23) 87.6(3) ?
Re(2) Re(2) O(23) 59.7(3) ?
O(23) Re(2) O(23) 27.8(6) ?
Re(2) Re(2) O(22) 168.5(3) ?
O(23) Re(2) O(22) 81.2(4) ?
O(23) Re(2) O(22) 109.1(4) ?
Re(2) Re(2) O(21) 74.34(6) ?
O(23) Re(2) O(21) 123.7(4) ?
O(23) Re(2) O(21) 110.7(3) ?
O(22) Re(2) O(21) 110.0(3) ?
Re(2) Re(2) Re(1) 79.391(11) ?
O(23) Re(2) Re(1) 121.1(3) ?
O(23) Re(2) Re(1) 111.1(3) ?
O(22) Re(2) Re(1) 108.5(3) ?
O(21) Re(2) Re(1) 107.5(2) ?
C(901) Cl(91) C(901) 34.7(13) ?
C(901) Cl(92) C(901) 36.0(12) ?
C(1B) P(1) C(121) 104.6(3) ?
C(1B) P(1) C(111) 102.7(3) ?
C(121) P(1) C(111) 110.7(3) ?
C(1B) P(1) Re(1) 95.1(2) ?
C(121) P(1) Re(1) 120.8(2) ?
C(111) P(1) Re(1) 118.4(2) ?
C(2B) P(2) C(221) 105.2(4) ?
C(2B) P(2) C(211) 101.6(3) ?
C(221) P(2) C(211) 109.5(3) ?
C(2B) P(2) Re(1) 93.9(2) ?
C(221) P(2) Re(1) 118.9(2) ?
C(211) P(2) Re(1) 122.7(2) ?
Re(2) O(21) Re(2) 31.32(11) ?
O(23) O(23) Re(2) 92.4(3) ?
O(23) O(23) Re(2) 59.7(3) ?
Re(2) O(23) Re(2) 32.73(17) ?
P(1) C(1B) P(1) 96.3(4) ?
P(2) C(2B) P(2) 98.2(4) ?
C(112) C(111) C(116) 109.4(5) ?
C(112) C(111) P(1) 117.0(4) ?
C(116) C(111) P(1) 115.0(4) ?
C(111) C(112) C(113) 109.8(5) ?
C(114) C(113) C(112) 111.8(6) ?
C(113) C(114) C(115) 111.6(6) ?
C(116) C(115) C(114) 111.3(6) ?
C(115) C(116) C(111) 109.8(5) ?
C(126) C(121) C(122) 110.3(6) ?
C(126) C(121) P(1) 119.0(5) ?
C(122) C(121) P(1) 112.2(4) ?
C(121) C(122) C(123) 110.2(6) ?
C(124) C(123) C(122) 111.5(7) ?
C(123) C(124) C(125) 111.9(6) ?
C(124) C(125) C(126) 112.4(7) ?
C(121) C(126) C(125) 109.1(6) ?
C(212) C(211) C(216) 109.1(5) ?
C(212) C(211) P(2) 116.9(4) ?
C(216) C(211) P(2) 115.3(5) ?
C(213) C(212) C(211) 109.6(5) ?
C(212) C(213) C(214) 110.9(6) ?
C(215) C(214) C(213) 111.7(6) ?
C(214) C(215) C(216) 112.3(6) ?
C(215) C(216) C(211) 110.8(6) ?
C(226) C(221) C(222) 110.2(10) ?
C(226) C(221) P(2) 112.6(6) ?
C(222) C(221) P(2) 116.6(5) ?
C(221) C(222) C(223) 110.3(7) ?
C(224) C(223) C(222) 108.6(12) ?
C(225) C(224) C(223) 113.0(9) ?
C(224) C(225) C(226) 112.5(13) ?
C(221) C(226) C(225) 109.8(8) ?
Cl(92) C(901) Cl(91) 119.0(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re(1) P(1) 2.4710(15) ?
Re(1) P(1) 2.4710(15) ?
Re(1) P(2) 2.4872(15) ?
Re(1) P(2) 2.4873(15) ?
Re(1) Cl(1) 2.493(2) ?
Re(1) Re(2) 2.5398(6) ?
Re(1) Re(2) 2.5398(6) ?
Re(2) Re(2) 0.9351(9) ?
Re(2) O(23) 1.493(8) ?
Re(2) O(23) 1.728(8) ?
Re(2) O(22) 1.731(8) ?
Re(2) O(21) 1.732(6) ?
Cl(91) C(901) 1.711(16) ?
Cl(91) C(901) 1.711(16) ?
Cl(92) C(901) 1.650(16) ?
Cl(92) C(901) 1.650(16) ?
P(1) C(1B) 1.845(6) ?
P(1) C(121) 1.851(7) ?
P(1) C(111) 1.857(6) ?
P(2) C(2B) 1.834(6) ?
P(2) C(221) 1.857(7) ?
P(2) C(211) 1.863(7) ?
O(21) Re(2) 1.732(6) ?
O(23) O(23) 0.808(17) ?
O(23) Re(2) 1.728(8) ?
C(1B) P(1) 1.845(6) ?
C(2B) P(2) 1.834(6) ?
C(111) C(112) 1.521(9) ?
C(111) C(116) 1.545(8) ?
C(112) C(113) 1.540(9) ?
C(113) C(114) 1.529(10) ?
C(114) C(115) 1.539(10) ?
C(115) C(116) 1.520(9) ?
C(121) C(126) 1.519(9) ?
C(121) C(122) 1.528(9) ?
C(122) C(123) 1.535(9) ?
C(123) C(124) 1.508(12) ?
C(124) C(125) 1.510(14) ?
C(125) C(126) 1.540(10) ?
C(211) C(212) 1.527(9) ?
C(211) C(216) 1.532(9) ?
C(212) C(213) 1.523(9) ?
C(213) C(214) 1.524(10) ?
C(214) C(215) 1.514(11) ?
C(215) C(216) 1.518(10) ?
C(221) C(226) 1.495(11) ?
C(221) C(222) 1.505(11) ?
C(222) C(223) 1.560(12) ?
C(223) C(224) 1.48(2) ?
C(224) C(225) 1.46(2) ?
C(225) C(226) 1.543(12) ?
