#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317461.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_4317461
loop_
_publ_author_name
'Shan-Ming Kuang'
'Phillip E. Fanwick'
'Richard A. Walton'
_publ_section_title
;
 Unsymmetrical Dirhenium Complexes That Contain [Re2]6+ and [Re2]5+ Cores
 Complexed by Tridentate Ligands with P2O and P2N Donor Sets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              405
_journal_page_last               412
_journal_paper_doi               10.1021/ic010983g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C46 H34 Cl4 N O3 P2 Re2'
_chemical_formula_weight         1224.95
_chemical_name_systematic        ' ?'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7371(3)
_cell_length_b                   14.5258(4)
_cell_length_c                   22.7450(4)
_cell_measurement_reflns_used    25011
_cell_measurement_temperature    149
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4208.20(17)
_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)
     PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF92,_Beurskins,_1992)
_diffrn_ambient_temperature      149
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25011
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    6.201
_exptl_absorpt_correction_T_max  0.3945
_exptl_absorpt_correction_T_min  0.3293
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.93
_exptl_crystal_description       plate
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.52
_refine_diff_density_min         -1.50
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9419
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[σ²(Fo²)+(0.0245P)²+0.0000P] where P=(Fo²+2Fc²)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.077
_reflns_number_gt                8628
_reflns_number_total             9439
_reflns_threshold_expression     >2.0σ(I)
_cod_data_source_file            ic010983g_6.cif
_cod_data_source_block           KSM61
_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        4208.2(3)
_cod_original_formula_sum        'C46 H34 Cl4 N1 O3 P2 Re2'
_cod_database_code               4317461
#BEGIN Tags that were not found in dictionaries:
_reflns_friedl_coverage          0.8912
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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) 0.74402(2) 1.00559(2) 0.819142(11) 0.01804(7) Uani ?
Re(2) 0.88193(2) 0.95442(2) 0.766380(12) 0.01981(7) Uani ?
Cl(11) 0.66724(14) 1.12642(13) 0.76491(9) 0.0255(5) Uani ?
Cl(21) 1.02740(18) 1.0293(2) 0.79714(10) 0.0485(8) Uani ?
Cl(22) 0.87928(15) 1.04901(15) 0.68406(8) 0.0317(5) Uani ?
Cl(23) 0.83628(18) 0.82989(16) 0.70813(9) 0.0385(6) Uani ?
P(1) 0.82016(16) 1.11688(14) 0.88665(8) 0.0198(5) Uani ?
P(2) 0.60086(15) 0.90683(15) 0.78754(8) 0.0215(5) Uani ?
O(1) 0.7706(4) 0.9046(3) 0.88288(19) 0.0177(14) Uani ?
O(2) 0.9070(4) 0.8546(4) 0.8298(2) 0.0253(15) Uani ?
O(12) 0.6058(4) 1.0349(4) 0.8856(2) 0.0253(15) Uani ?
N(4) 0.8810(7) 0.6070(5) 0.9828(3) 0.040(2) Uani ?
C(0) 0.8429(6) 0.8467(5) 0.8736(3) 0.020(2) Uani ?
C(1) 0.8576(6) 0.7680(6) 0.9149(3) 0.025(2) Uani ?
C(2) 0.9145(7) 0.6950(7) 0.8941(4) 0.036(3) Uani ?
C(3) 0.9235(7) 0.6176(7) 0.9302(4) 0.039(3) Uani ?
C(5) 0.8275(7) 0.6801(7) 1.0045(4) 0.034(3) Uani ?
C(6) 0.7896(7) 0.6719(7) 1.0622(4) 0.043(3) Uani ?
C(7) 0.7358(9) 0.7432(7) 1.0887(4) 0.051(3) Uani ?
C(8) 0.7201(8) 0.8271(7) 1.0569(4) 0.047(3) Uani ?
C(9) 0.7561(8) 0.8374(6) 1.0010(3) 0.040(3) Uani ?
C(10) 0.8129(7) 0.7648(6) 0.9727(4) 0.026(2) Uani ?
C(111) 0.7289(6) 1.1099(5) 0.9476(3) 0.022(2) Uani ?
C(112) 0.6313(6) 1.0697(5) 0.9423(3) 0.0217(18) Uani ?
C(113) 0.5608(6) 1.0557(7) 0.9885(3) 0.030(2) Uani ?
C(114) 0.5942(7) 1.0870(6) 1.0446(4) 0.036(3) Uani ?
C(115) 0.6919(7) 1.1251(6) 1.0528(3) 0.032(2) Uani ?
C(116) 0.7582(7) 1.1371(6) 1.0050(3) 0.029(2) Uani ?
C(121) 0.9475(6) 1.0953(6) 0.9227(3) 0.024(2) Uani ?
C(122) 0.9661(6) 1.0104(6) 0.9473(3) 0.028(2) Uani ?
C(123) 1.0647(7) 0.9873(7) 0.9696(4) 0.033(2) Uani ?
C(124) 1.1429(6) 1.0514(7) 0.9686(3) 0.032(2) Uani ?
C(125) 1.1229(7) 1.1387(6) 0.9454(3) 0.029(2) Uani ?
C(126) 1.0264(6) 1.1604(6) 0.9212(3) 0.029(2) Uani ?
C(131) 0.8252(6) 1.2369(6) 0.8643(3) 0.023(2) Uani ?
C(132) 0.7992(6) 1.3089(6) 0.9008(4) 0.029(2) Uani ?
C(133) 0.8089(7) 1.4000(6) 0.8816(4) 0.034(2) Uani ?
C(134) 0.8453(6) 1.4181(6) 0.8255(4) 0.033(2) Uani ?
C(135) 0.8712(7) 1.3454(6) 0.7893(4) 0.031(2) Uani ?
C(136) 0.8616(6) 1.2557(6) 0.8076(3) 0.029(2) Uani ?
C(211) 0.4883(6) 0.9693(6) 0.8167(3) 0.028(2) Uani ?
C(212) 0.5030(6) 1.0329(6) 0.8616(3) 0.027(2) Uani ?
C(213) 0.4239(6) 1.0922(7) 0.8797(4) 0.032(2) Uani ?
C(214) 0.3287(7) 1.0856(8) 0.8523(4) 0.048(3) Uani ?
C(215) 0.3079(7) 1.0201(8) 0.8100(4) 0.050(3) Uani ?
C(216) 0.3887(6) 0.9634(7) 0.7922(3) 0.035(2) Uani ?
C(221) 0.5662(6) 0.8866(6) 0.7102(3) 0.025(2) Uani ?
C(222) 0.6008(5) 0.9477(6) 0.6682(3) 0.025(2) Uani ?
C(223) 0.5678(6) 0.9364(7) 0.6104(3) 0.034(3) Uani ?
C(224) 0.5007(7) 0.8654(7) 0.5966(4) 0.039(3) Uani ?
C(225) 0.4668(7) 0.8052(7) 0.6382(4) 0.035(3) Uani ?
C(226) 0.4990(6) 0.8140(6) 0.6958(3) 0.032(2) Uani ?
C(231) 0.5970(6) 0.7950(5) 0.8234(3) 0.027(2) Uani ?
C(232) 0.6483(7) 0.7203(6) 0.8009(4) 0.034(3) Uani ?
C(233) 0.6517(8) 0.6378(7) 0.8304(4) 0.043(3) Uani ?
C(234) 0.6040(8) 0.6286(7) 0.8847(4) 0.043(3) Uani ?
C(235) 0.5535(9) 0.7047(8) 0.9088(5) 0.060(4) Uani ?
C(236) 0.5489(8) 0.7863(7) 0.8788(4) 0.048(3) Uani ?
H(2) 0.9461 0.6968 0.8572 0.0470 Uiso calc
H(3) 0.9633 0.5688 0.9158 0.0510 Uiso calc
H(6) 0.8010 0.6177 1.0830 0.0570 Uiso calc
H(7) 0.7099 0.7368 1.1267 0.0660 Uiso calc
H(8) 0.6848 0.8755 1.0749 0.0610 Uiso calc
H(9) 0.7437 0.8921 0.9809 0.0510 Uiso calc
H(113) 0.4960 1.0276 0.9829 0.0390 Uiso calc
H(114) 0.5489 1.0816 1.0765 0.0470 Uiso calc
H(115) 0.7135 1.1427 1.0902 0.0420 Uiso calc
H(116) 0.8237 1.1638 1.0109 0.0380 Uiso calc
H(122) 0.9120 0.9675 0.9490 0.0360 Uiso calc
H(123) 1.0769 0.9290 0.9850 0.0430 Uiso calc
H(124) 1.2090 1.0371 0.9833 0.0420 Uiso calc
H(125) 1.1755 1.1831 0.9462 0.0370 Uiso calc
H(126) 1.0149 1.2178 0.9043 0.0370 Uiso calc
H(132) 0.7750 1.2969 0.9386 0.0380 Uiso calc
H(133) 0.7909 1.4483 0.9065 0.0440 Uiso calc
H(134) 0.8522 1.4784 0.8123 0.0430 Uiso calc
H(135) 0.8957 1.3574 0.7516 0.0410 Uiso calc
H(136) 0.8793 1.2077 0.7824 0.0380 Uiso calc
H(213) 0.4353 1.1349 0.9095 0.0410 Uiso calc
H(214) 0.2760 1.1269 0.8625 0.0620 Uiso calc
H(215) 0.2411 1.0142 0.7940 0.0650 Uiso calc
H(216) 0.3761 0.9201 0.7629 0.0450 Uiso calc
H(222) 0.6455 0.9957 0.6783 0.0330 Uiso calc
H(223) 0.5910 0.9765 0.5813 0.0450 Uiso calc
H(224) 0.4781 0.8585 0.5580 0.0510 Uiso calc
H(225) 0.4215 0.7577 0.6277 0.0460 Uiso calc
H(226) 0.4766 0.7726 0.7243 0.0420 Uiso calc
H(232) 0.6819 0.7254 0.7648 0.0440 Uiso calc
H(233) 0.6863 0.5878 0.8137 0.0550 Uiso calc
H(234) 0.6056 0.5728 0.9046 0.0570 Uiso calc
H(235) 0.5226 0.7001 0.9457 0.0770 Uiso calc
H(236) 0.5138 0.8363 0.8951 0.0630 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
O(1) Re(1) Re(2) 90.67(13) ?
O(1) Re(1) Cl(11) 162.29(13) ?
Re(2) Re(1) Cl(11) 106.87(5) ?
O(1) Re(1) O(12) 78.63(18) ?
Re(2) Re(1) O(12) 169.23(13) ?
Cl(11) Re(1) O(12) 83.78(14) ?
O(1) Re(1) P(2) 84.97(14) ?
Re(2) Re(1) P(2) 103.46(5) ?
Cl(11) Re(1) P(2) 88.48(7) ?
O(12) Re(1) P(2) 74.70(14) ?
O(1) Re(1) P(1) 87.93(14) ?
Re(2) Re(1) P(1) 104.16(5) ?
Cl(11) Re(1) P(1) 90.05(7) ?
O(12) Re(1) P(1) 76.88(14) ?
P(2) Re(1) P(1) 151.53(7) ?
O(2) Re(2) Re(1) 88.85(14) ?
O(2) Re(2) Cl(21) 89.72(16) ?
Re(1) Re(2) Cl(21) 108.39(6) ?
O(2) Re(2) Cl(23) 83.71(16) ?
Re(1) Re(2) Cl(23) 111.50(6) ?
Cl(21) Re(2) Cl(23) 139.37(9) ?
O(2) Re(2) Cl(22) 168.07(14) ?
Re(1) Re(2) Cl(22) 102.88(5) ?
Cl(21) Re(2) Cl(22) 88.66(9) ?
Cl(23) Re(2) Cl(22) 89.84(8) ?
C(111) P(1) C(131) 106.9(4) ?
C(111) P(1) C(121) 102.3(3) ?
C(131) P(1) C(121) 104.8(4) ?
C(111) P(1) Re(1) 101.0(3) ?
C(131) P(1) Re(1) 118.4(3) ?
C(121) P(1) Re(1) 121.3(3) ?
C(231) P(2) C(211) 105.1(4) ?
C(231) P(2) C(221) 106.3(4) ?
C(211) P(2) C(221) 103.8(4) ?
C(231) P(2) Re(1) 114.5(3) ?
C(211) P(2) Re(1) 100.9(3) ?
C(221) P(2) Re(1) 123.9(3) ?
C(0) O(1) Re(1) 118.0(4) ?
C(0) O(2) Re(2) 120.1(5) ?
C(212) O(12) C(112) 124.6(5) ?
C(212) O(12) Re(1) 115.9(4) ?
C(112) O(12) Re(1) 118.3(4) ?
C(3) N(4) C(5) 116.4(8) ?
O(1) C(0) O(2) 122.0(7) ?
O(1) C(0) C(1) 119.8(6) ?
O(2) C(0) C(1) 118.2(7) ?
C(2) C(1) C(10) 120.1(8) ?
C(2) C(1) C(0) 116.3(7) ?
C(10) C(1) C(0) 123.5(7) ?
C(1) C(2) C(3) 117.6(8) ?
N(4) C(3) C(2) 126.3(8) ?
N(4) C(5) C(6) 116.6(8) ?
N(4) C(5) C(10) 123.4(8) ?
C(6) C(5) C(10) 119.9(9) ?
C(7) C(6) C(5) 121.0(8) ?
C(6) C(7) C(8) 119.3(9) ?
C(9) C(8) C(7) 121.2(9) ?
C(8) C(9) C(10) 120.6(8) ?
C(9) C(10) C(1) 126.1(8) ?
C(9) C(10) C(5) 117.9(8) ?
C(1) C(10) C(5) 116.0(8) ?
C(112) C(111) C(116) 115.9(7) ?
C(112) C(111) P(1) 122.3(6) ?
C(116) C(111) P(1) 121.5(6) ?
C(111) C(112) C(113) 125.1(7) ?
C(111) C(112) O(12) 115.9(6) ?
C(113) C(112) O(12) 118.9(7) ?
C(112) C(113) C(114) 115.9(8) ?
C(115) C(114) C(113) 121.5(7) ?
C(114) C(115) C(116) 119.7(8) ?
C(115) C(116) C(111) 121.9(8) ?
C(122) C(121) C(126) 120.0(7) ?
C(122) C(121) P(1) 119.0(6) ?
C(126) C(121) P(1) 120.8(6) ?
C(121) C(122) C(123) 121.2(8) ?
C(124) C(123) C(122) 119.2(8) ?
C(123) C(124) C(125) 119.5(8) ?
C(126) C(125) C(124) 121.3(8) ?
C(125) C(126) C(121) 118.7(8) ?
C(132) C(131) C(136) 119.2(8) ?
C(132) C(131) P(1) 123.5(6) ?
C(136) C(131) P(1) 117.3(6) ?
C(131) C(132) C(133) 120.6(8) ?
C(134) C(133) C(132) 119.8(8) ?
C(135) C(134) C(133) 119.0(8) ?
C(136) C(135) C(134) 121.7(8) ?
C(135) C(136) C(131) 119.6(8) ?
C(216) C(211) C(212) 117.4(7) ?
C(216) C(211) P(2) 122.8(6) ?
C(212) C(211) P(2) 119.5(6) ?
C(211) C(212) C(213) 122.2(7) ?
C(211) C(212) O(12) 114.9(7) ?
C(213) C(212) O(12) 122.9(7) ?
C(214) C(213) C(212) 117.7(9) ?
C(213) C(214) C(215) 122.4(9) ?
C(214) C(215) C(216) 118.4(8) ?
C(215) C(216) C(211) 121.8(8) ?
C(222) C(221) C(226) 121.3(7) ?
C(222) C(221) P(2) 119.0(6) ?
C(226) C(221) P(2) 119.5(6) ?
C(221) C(222) C(223) 118.9(8) ?
C(224) C(223) C(222) 119.5(8) ?
C(225) C(224) C(223) 121.4(8) ?
C(224) C(225) C(226) 120.5(9) ?
C(225) C(226) C(221) 118.3(8) ?
C(232) C(231) C(236) 118.2(8) ?
C(232) C(231) P(2) 121.9(6) ?
C(236) C(231) P(2) 119.6(7) ?
C(231) C(232) C(233) 121.7(8) ?
C(232) C(233) C(234) 120.4(9) ?
C(233) C(234) C(235) 118.6(9) ?
C(236) C(235) C(234) 120.7(9) ?
C(235) C(236) C(231) 120.4(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re(1) O(1) 2.090(5) ?
Re(1) Re(2) 2.2536(4) ?
Re(1) Cl(11) 2.3577(18) ?
Re(1) O(12) 2.360(4) ?
Re(1) P(2) 2.429(2) ?
Re(1) P(1) 2.431(2) ?
Re(2) O(2) 2.070(5) ?
Re(2) Cl(21) 2.260(2) ?
Re(2) Cl(23) 2.316(2) ?
Re(2) Cl(22) 2.3227(18) ?
P(1) C(111) 1.812(7) ?
P(1) C(131) 1.817(8) ?
P(1) C(121) 1.845(8) ?
P(2) C(231) 1.818(8) ?
P(2) C(211) 1.822(8) ?
P(2) C(221) 1.838(8) ?
O(1) C(0) 1.265(9) ?
O(2) C(0) 1.293(8) ?
O(12) C(212) 1.419(9) ?
O(12) C(112) 1.422(8) ?
N(4) C(3) 1.323(10) ?
N(4) C(5) 1.355(11) ?
C(0) C(1) 1.491(10) ?
C(1) C(2) 1.369(11) ?
C(1) C(10) 1.434(11) ?
C(2) C(3) 1.396(12) ?
C(5) C(6) 1.403(12) ?
C(5) C(10) 1.440(12) ?
C(6) C(7) 1.380(14) ?
C(7) C(8) 1.430(13) ?
C(8) C(9) 1.361(11) ?
C(9) C(10) 1.432(12) ?
C(111) C(112) 1.379(11) ?
C(111) C(116) 1.413(10) ?
C(112) C(113) 1.398(10) ?
C(113) C(114) 1.419(12) ?
C(114) C(115) 1.375(12) ?
C(115) C(116) 1.387(11) ?
C(121) C(122) 1.374(11) ?
C(121) C(126) 1.380(11) ?
C(122) C(123) 1.396(11) ?
C(123) C(124) 1.363(12) ?
C(124) C(125) 1.397(12) ?
C(125) C(126) 1.382(11) ?
C(131) C(132) 1.377(11) ?
C(131) C(136) 1.396(11) ?
C(132) C(133) 1.399(12) ?
C(133) C(134) 1.384(12) ?
C(134) C(135) 1.378(11) ?
C(135) C(136) 1.373(11) ?
C(211) C(216) 1.388(11) ?
C(211) C(212) 1.389(11) ?
C(212) C(213) 1.388(11) ?
C(213) C(214) 1.368(12) ?
C(214) C(215) 1.378(15) ?
C(215) C(216) 1.379(11) ?
C(221) C(222) 1.376(10) ?
C(221) C(226) 1.397(11) ?
C(222) C(223) 1.389(10) ?
C(223) C(224) 1.375(13) ?
C(224) C(225) 1.358(13) ?
C(225) C(226) 1.379(11) ?
C(231) C(232) 1.367(11) ?
C(231) C(236) 1.406(12) ?
C(232) C(233) 1.373(12) ?
C(233) C(234) 1.383(12) ?
C(234) C(235) 1.391(14) ?
C(235) C(236) 1.369(13) ?
