#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/51/7115125.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_7115125
loop_
_publ_author_name
'Bhattacharyya, Sibaprasad'
'Chakraborty, Indranil'
'Dirghangi, Bimal Kumar'
'Chakravorty, Animesh'
_publ_section_title
;
 Oxygen atom transfer from RevO to tertiary diphosphines: spacer length
 and chemical differentiation of products
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1813
_journal_paper_doi               10.1039/b004565i
_journal_year                    2000
_chemical_formula_sum            'C35 H31 Cl4 N4 O2 P2 Re'
_chemical_formula_weight         929.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.353(11)
_cell_length_b                   12.730(6)
_cell_length_c                   16.840(7)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     7331(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       'ω scans'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5705
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.732
_exptl_absorpt_correction_T_max  0.242
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.115
_refine_ls_goodness_of_fit_obs   1.129
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.129
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_obs          0.0585
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0374P)²+80.4023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1369
_refine_ls_wR_factor_obs         0.1060
_reflns_number_observed          3386
_reflns_number_total             5422
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004565i.txt
_cod_data_source_block           709re
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+80.4023P] 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^)+(0.0374P)^2^+80.4023P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        7331.5(51)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7115125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Re Re 0.087663(15) 0.29803(4) -0.02101(3) 0.0540(2) Uani 1 d .
Cl1 Cl 0.12880(13) 0.4147(3) 0.0727(3) 0.0959(14) Uani 1 d .
Cl2 Cl 0.05719(10) 0.2506(3) 0.0840(2) 0.0770(11) Uani 1 d .
Cl3 Cl 0.12343(10) 0.3366(3) -0.1179(2) 0.0789(11) Uani 1 d .
P1 P 0.14685(9) 0.1041(3) 0.0828(2) 0.0534(9) Uani 1 d .
P2 P 0.18710(9) 0.1355(3) 0.2718(2) 0.0509(8) Uani 1 d .
O1 O 0.1232(2) 0.1716(6) 0.0131(5) 0.060(2) Uani 1 d .
O2 O 0.1825(3) 0.0256(6) 0.2920(5) 0.067(2) Uani 1 d .
N1 N 0.0481(3) 0.4093(9) -0.0637(7) 0.065(3) Uani 1 d .
N2 N -0.0110(4) 0.4525(12) -0.1422(9) 0.089(4) Uani 1 d .
N3 N 0.0113(3) 0.2724(10) -0.1385(7) 0.072(3) Uani 1 d .
N4 N 0.0455(3) 0.2254(8) -0.1030(6) 0.056(3) Uani 1 d .
C1 C 0.0427(5) 0.5175(12) -0.0571(10) 0.088(5) Uani 1 d .
H1A H 0.0604(5) 0.5643(12) -0.0253(10) 0.106 Uiso 1 calc R
C2 C 0.0071(6) 0.5416(16) -0.1052(13) 0.107(6) Uani 1 d .
H2A H -0.0036(6) 0.6087(16) -0.1123(13) 0.128 Uiso 1 calc R
C3 C 0.0151(5) 0.3735(12) -0.1149(10) 0.071(4) Uani 1 d .
C4 C -0.0491(4) 0.4438(14) -0.1993(10) 0.114(7) Uani 1 d .
H4A H -0.0612(4) 0.5118(14) -0.2076(10) 0.171 Uiso 1 calc R
H4B H -0.0651(4) 0.3968(14) -0.1774(10) 0.171 Uiso 1 calc R
H4C H -0.0463(4) 0.4171(14) -0.2507(10) 0.171 Uiso 1 calc R
C5 C 0.0469(3) 0.1138(11) -0.1224(8) 0.062(4) Uani 1 d .
C6 C 0.0175(5) 0.0495(14) -0.1148(12) 0.114(7) Uani 1 d .
H6A H -0.0031(5) 0.0769(14) -0.0961(12) 0.137 Uiso 1 calc R
C7 C 0.0173(5) -0.0554(13) -0.1343(12) 0.110(6) Uani 1 d .
H7A H -0.0033(5) -0.0987(13) -0.1305(12) 0.132 Uiso 1 calc R
C8 C 0.0488(5) -0.0946(13) -0.1598(11) 0.096(5) Uani 1 d .
C9 C 0.0790(5) -0.0304(12) -0.1644(9) 0.076(4) Uani 1 d .
H9A H 0.1002(5) -0.0582(12) -0.1806(9) 0.091 Uiso 1 calc R
C10 C 0.0789(4) 0.0766(11) -0.1453(8) 0.066(4) Uani 1 d .
H10A H 0.0996(4) 0.1204(11) -0.1480(8) 0.080 Uiso 1 calc R
Cl4 Cl 0.0512(2) -0.2263(4) -0.1833(4) 0.145(2) Uani 1 d .
C11 C 0.1224(4) -0.0153(10) 0.0907(8) 0.054(3) Uani 1 d .
C12 C 0.1037(5) -0.0360(16) 0.1479(11) 0.122(7) Uani 1 d .
H12A H 0.1038(5) 0.0136(16) 0.1885(11) 0.147 Uiso 1 calc R
C13 C 0.0835(5) -0.1314(20) 0.1485(12) 0.145(9) Uani 1 d .
H13A H 0.0723(5) -0.1449(20) 0.1918(12) 0.175 Uiso 1 calc R
C14 C 0.0799(5) -0.2028(14) 0.0894(12) 0.100(5) Uani 1 d .
H14A H 0.0643(5) -0.2622(14) 0.0873(12) 0.120 Uiso 1 calc R
C15 C 0.1001(6) -0.1839(11) 0.0327(13) 0.108(6) Uani 1 d .
H15A H 0.0989(6) -0.2329(11) -0.0088(13) 0.129 Uiso 1 calc R
C16 C 0.1236(5) -0.0908(14) 0.0339(10) 0.103(6) Uani 1 d .
H16A H 0.1390(5) -0.0826(14) -0.0029(10) 0.123 Uiso 1 calc R
C17 C 0.1925(3) 0.0760(10) 0.0612(8) 0.055(3) Uani 1 d .
C18 C 0.2175(4) 0.0006(11) 0.1039(8) 0.065(4) Uani 1 d .
H18A H 0.2098(4) -0.0404(11) 0.1428(8) 0.078 Uiso 1 calc R
C19 C 0.2538(4) -0.0143(13) 0.0894(9) 0.077(4) Uani 1 d .
H19A H 0.2709(4) -0.0646(13) 0.1184(9) 0.093 Uiso 1 calc R
C20 C 0.2642(4) 0.0466(13) 0.0313(10) 0.083(5) Uani 1 d .
H20A H 0.2889(4) 0.0384(13) 0.0227(10) 0.100 Uiso 1 calc R
C21 C 0.2397(4) 0.1182(12) -0.0140(10) 0.084(5) Uani 1 d .
H21A H 0.2472(4) 0.1563(12) -0.0547(10) 0.100 Uiso 1 calc R
C22 C 0.2036(4) 0.1341(11) 0.0010(9) 0.074(4) Uani 1 d .
H22A H 0.1866(4) 0.1838(11) -0.0292(9) 0.089 Uiso 1 calc R
C23 C 0.1542(3) 0.1780(9) 0.1772(7) 0.055(3) Uani 1 d .
H23A H 0.1626(3) 0.2478(9) 0.1659(7) 0.065 Uiso 1 calc R
H23B H 0.1287(3) 0.1861(9) 0.1881(7) 0.065 Uiso 1 calc R
C24 C 0.2363(3) 0.1666(10) 0.2665(7) 0.048(3) Uani 1 d .
C25 C 0.2654(4) 0.0927(13) 0.2939(9) 0.084(5) Uani 1 d .
H25A H 0.2592(4) 0.0283(13) 0.3134(9) 0.101 Uiso 1 calc R
C26 C 0.3033(5) 0.1136(16) 0.2926(10) 0.096(5) Uani 1 d .
H26A H 0.3227(5) 0.0634(16) 0.3110(10) 0.115 Uiso 1 calc R
C27 C 0.3125(5) 0.2075(19) 0.2646(10) 0.100(6) Uani 1 d .
H27A H 0.3384(5) 0.2219(19) 0.2654(10) 0.120 Uiso 1 calc R
C28 C 0.2847(5) 0.2811(15) 0.2354(9) 0.088(5) Uani 1 d .
H28A H 0.2912(5) 0.3442(15) 0.2145(9) 0.106 Uiso 1 calc R
C29 C 0.2463(4) 0.2609(12) 0.2371(8) 0.072(4) Uani 1 d .
H29A H 0.2271(4) 0.3115(12) 0.2182(8) 0.087 Uiso 1 calc R
C30 C 0.1768(4) 0.2246(10) 0.3457(8) 0.055(3) Uani 1 d .
C31 C 0.1949(5) 0.2009(13) 0.4282(9) 0.093(5) Uani 1 d .
H31A H 0.2104(5) 0.1411(13) 0.4413(9) 0.111 Uiso 1 calc R
C32 C 0.1896(6) 0.2667(14) 0.4892(10) 0.102(6) Uani 1 d .
H32A H 0.2023(6) 0.2525(14) 0.5436(10) 0.123 Uiso 1 calc R
C33 C 0.1653(6) 0.3549(14) 0.4704(13) 0.104(7) Uani 1 d .
H33A H 0.1609(6) 0.3973(14) 0.5120(13) 0.124 Uiso 1 calc R
C34 C 0.1485(5) 0.3773(13) 0.3917(12) 0.087(5) Uani 1 d .
H34A H 0.1329(5) 0.4368(13) 0.3787(12) 0.105 Uiso 1 calc R
C35 C 0.1541(4) 0.3143(12) 0.3303(9) 0.074(4) Uani 1 d .
H35A H 0.1423(4) 0.3322(12) 0.2762(9) 0.089 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'
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_publ_flag
N4 Re N1 75.2(4) y
N4 Re O1 97.5(4) y
N1 Re O1 172.7(4) y
N4 Re Cl3 93.2(3) y
N1 Re Cl3 93.0(3) y
O1 Re Cl3 87.7(3) y
N4 Re Cl2 89.8(3) y
N1 Re Cl2 92.3(3) y
O1 Re Cl2 87.3(3) y
Cl3 Re Cl2 174.43(13) y
N4 Re Cl1 168.0(3) y
N1 Re Cl1 92.9(4) y
O1 Re Cl1 94.4(2) y
Cl3 Re Cl1 89.08(15) y
Cl2 Re Cl1 88.9(2) y
O1 P1 C11 111.1(5) ?
O1 P1 C17 107.7(6) ?
C11 P1 C17 109.1(6) ?
O1 P1 C23 108.2(5) ?
C11 P1 C23 110.2(6) ?
C17 P1 C23 110.4(5) ?
O2 P2 C30 113.1(6) ?
O2 P2 C23 114.2(6) ?
C30 P2 C23 103.0(6) ?
O2 P2 C24 112.7(6) ?
C30 P2 C24 105.3(5) ?
C23 P2 C24 107.7(6) ?
P1 O1 Re 147.5(5) y
C3 N1 C1 105.7(13) ?
C3 N1 Re 114.0(9) ?
C1 N1 Re 140.3(12) ?
C3 N2 C2 104.9(14) ?
C3 N2 C4 127.2(17) ?
C2 N2 C4 127.8(15) ?
N4 N3 C3 106.5(11) ?
N3 N4 C5 114.3(10) ?
N3 N4 Re 122.3(8) ?
C5 N4 Re 123.0(7) ?
C2 C1 N1 107.6(17) ?
C1 C2 N2 110.0(16) ?
N1 C3 N3 121.4(12) ?
N1 C3 N2 111.7(15) ?
N3 C3 N2 126.7(16) ?
C6 C5 C10 121.8(14) ?
C6 C5 N4 119.7(12) ?
C10 C5 N4 118.5(12) ?
C5 C6 C7 121.4(16) ?
C6 C7 C8 118.0(16) ?
C9 C8 C7 120.3(15) ?
C9 C8 Cl4 119.0(13) ?
C7 C8 Cl4 120.7(15) ?
C8 C9 C10 121.6(14) ?
C5 C10 C9 116.9(14) ?
C12 C11 C16 118.6(15) ?
C12 C11 P1 124.6(12) ?
C16 C11 P1 116.8(11) ?
C11 C12 C13 121.6(16) ?
C14 C13 C12 122.4(17) ?
C13 C14 C15 116.1(17) ?
C14 C15 C16 122.7(17) ?
C11 C16 C15 118.0(15) ?
C18 C17 C22 119.3(12) ?
C18 C17 P1 121.9(11) ?
C22 C17 P1 118.8(10) ?
C17 C18 C19 120.4(13) ?
C20 C19 C18 118.5(14) ?
C21 C20 C19 122.5(13) ?
C20 C21 C22 119.1(14) ?
C21 C22 C17 120.1(13) ?
P2 C23 P1 122.5(6) ?
C29 C24 C25 118.3(13) ?
C29 C24 P2 123.1(10) ?
C25 C24 P2 118.6(11) ?
C26 C25 C24 120.7(16) ?
C27 C26 C25 119.8(17) ?
C26 C27 C28 121.3(16) ?
C27 C28 C29 119.2(16) ?
C24 C29 C28 120.7(14) ?
C35 C30 C31 117.4(12) ?
C35 C30 P2 127.2(10) ?
C31 C30 P2 115.4(10) ?
C32 C31 C30 119.4(16) ?
C31 C32 C33 120.8(17) ?
C34 C33 C32 119.2(16) ?
C33 C34 C35 120.8(17) ?
C34 C35 C30 122.3(14) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re N4 1.985(10) y
Re N1 1.993(11) y
Re O1 2.033(7) y
Re Cl3 2.356(4) y
Re Cl2 2.370(4) y
Re Cl1 2.377(4) y
P1 O1 1.523(8) y
P1 C11 1.770(13) ?
P1 C17 1.778(12) ?
P1 C23 1.808(11) ?
P2 O2 1.459(8) y
P2 C30 1.788(12) ?
P2 C23 1.801(11) ?
P2 C24 1.807(12) ?
N1 C3 1.34(2) ?
N1 C1 1.40(2) ?
N2 C3 1.36(2) ?
N2 C2 1.37(2) ?
N2 C4 1.45(2) ?
N3 N4 1.343(12) y
N3 C3 1.34(2) ?
N4 C5 1.46(2) ?
C1 C2 1.35(2) ?
C5 C6 1.36(2) ?
C5 C10 1.37(2) ?
C6 C7 1.38(2) ?
C7 C8 1.38(2) ?
C8 C9 1.36(2) ?
C8 Cl4 1.73(2) ?
C9 C10 1.40(2) ?
C11 C12 1.33(2) ?
C11 C16 1.36(2) ?
C12 C13 1.41(2) ?
C13 C14 1.33(2) ?
C14 C15 1.35(2) ?
C15 C16 1.44(2) ?
C17 C18 1.38(2) ?
C17 C22 1.39(2) ?
C18 C19 1.38(2) ?
C19 C20 1.37(2) ?
C20 C21 1.35(2) ?
C21 C22 1.38(2) ?
C24 C29 1.38(2) ?
C24 C25 1.39(2) ?
C25 C26 1.37(2) ?
C26 C27 1.35(2) ?
C27 C28 1.36(2) ?
C28 C29 1.39(2) ?
C30 C35 1.38(2) ?
C30 C31 1.41(2) ?
C31 C32 1.38(2) ?
C32 C33 1.40(2) ?
C33 C34 1.34(2) ?
C34 C35 1.36(2) ?
