#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:33:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179976 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/70/7027053.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027053
loop_
_publ_author_name
'Bhattacharyya, Sibaprasad'
'Banerjee, Sangeeta'
'Kumar Dirghangi, Bimal'
'Menon, Mahua'
'Chakravorty, Animesh'
_publ_section_title
;
 Synthesis, structure and redox behaviour of facial [ReIIIL(PPh3)Cl3] and
 its stereoretentive conversion to [ReIVL′(PPh3)Cl3] via metal
 promoted aldimine →  amide oxidation
 (L = pyridine-2-aldimine;
 L′ = pyridine-2-carboxamide)
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              155
_journal_paper_doi               10.1039/a806346j
_journal_year                    1999
_chemical_formula_sum            'C30 H25 Cl4 N2 O2 P Re'
_chemical_formula_weight         804.49
_chemical_name_systematic
; 
 ? 
;
_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     'Patterson Heavey atom Method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.26(4)
_cell_angle_beta                 88.11(5)
_cell_angle_gamma                67.40(4)
_cell_formula_units_Z            2
_cell_length_a                   9.994(6)
_cell_length_b                   11.617(6)
_cell_length_c                   15.135(9)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1572.5(17)
_computing_cell_refinement       'Siemens SHELXTL PLUS'
_computing_data_collection       'Siemens SHELXTL PLUS'
_computing_data_reduction        'Siemens SHELXTL PLUS'
_computing_molecular_graphics    'Siemens SHELXTL V 5.03'
_computing_publication_material  'Siemens SHELXTL V 5.03'
_computing_structure_refinement  'SHELXTL V 5.03 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V 5.03 (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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4733
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.285
_exptl_absorpt_correction_T_max  0.427
_exptl_absorpt_correction_T_min  0.227
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.087
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.153
_refine_ls_goodness_of_fit_obs   1.177
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.288
_refine_ls_restrained_S_obs      1.177
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0874P)²+3.1243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1554
_refine_ls_wR_factor_obs         0.1319
_reflns_number_observed          4054
_reflns_number_total             4663
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806346Jsup1.cif
_cod_data_source_block           fac-ReL4'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+3.1243P] 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^)+(0.0874P)^2^+3.1243P] 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        1572.5(16)
_cod_original_sg_symbol_H-M      P(-1)
_cod_database_code               7027053
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
Re Re 0.15241(4) 0.23317(3) 0.34727(3) 0.0351(2) Uani 1 d .
N1 N 0.3461(8) 0.2674(7) 0.3249(6) 0.040(2) Uani 1 d .
N2 N 0.0904(8) 0.3853(7) 0.2337(5) 0.038(2) Uani 1 d .
P P 0.2372(3) 0.0644(2) 0.2543(2) 0.0374(6) Uani 1 d .
O1 O 0.1716(8) 0.5238(7) 0.1344(5) 0.051(2) Uani 1 d .
Cl1 Cl 0.0965(3) 0.3758(3) 0.4412(2) 0.0541(7) Uani 1 d .
Cl2 Cl -0.0691(3) 0.2150(3) 0.3561(2) 0.0533(7) Uani 1 d .
Cl3 Cl 0.2637(3) 0.0594(2) 0.4724(2) 0.0468(6) Uani 1 d .
Cl4 Cl -0.5040(3) 0.6975(4) 0.0611(3) 0.0894(12) Uani 1 d .
C1 C 0.4736(12) 0.1989(12) 0.3741(9) 0.064(3) Uani 1 d .
H1A H 0.4832(12) 0.1303(12) 0.4233(9) 0.077 Uiso 1 calc R
C2 C 0.5859(14) 0.2325(15) 0.3501(12) 0.105(6) Uani 1 d .
H2A H 0.6732(14) 0.1866(15) 0.3851(12) 0.127 Uiso 1 calc R
C3 C 0.5801(13) 0.3325(13) 0.2756(11) 0.083(5) Uani 1 d .
H3A H 0.6592(13) 0.3554(13) 0.2619(11) 0.099 Uiso 1 calc R
C4 C 0.4525(12) 0.3942(12) 0.2244(9) 0.067(4) Uani 1 d .
H4A H 0.4431(12) 0.4585(12) 0.1721(9) 0.081 Uiso 1 calc R
C5 C 0.3380(10) 0.3603(9) 0.2511(7) 0.041(2) Uani 1 d .
C6 C 0.1899(10) 0.4329(9) 0.1991(7) 0.039(2) Uani 1 d .
C7 C -0.0545(10) 0.4590(9) 0.1932(6) 0.039(2) Uani 1 d .
C8 C -0.0889(11) 0.4606(10) 0.1055(7) 0.050(3) Uani 1 d .
H8A H -0.0181(11) 0.4123(10) 0.0728(7) 0.060 Uiso 1 calc R
C9 C -0.2279(12) 0.5335(12) 0.0652(8) 0.060(3) Uani 1 d .
H9A H -0.2507(12) 0.5334(12) 0.0061(8) 0.072 Uiso 1 calc R
C10 C -0.3302(10) 0.6049(11) 0.1129(8) 0.053(3) Uani 1 d .
C11 C -0.2995(12) 0.6051(11) 0.2010(8) 0.057(3) Uani 1 d .
H11A H -0.3701(12) 0.6545(11) 0.2333(8) 0.068 Uiso 1 calc R
C12 C -0.1621(12) 0.5306(11) 0.2396(8) 0.055(3) Uani 1 d .
H12A H -0.1410(12) 0.5286(11) 0.2995(8) 0.066 Uiso 1 calc R
C13 C 0.4343(12) 0.0081(10) 0.2513(8) 0.052(3) Uani 1 d .
C14 C 0.4993(14) 0.0850(14) 0.1918(9) 0.071(3) Uani 1 d .
H14A H 0.4404(14) 0.1607(14) 0.1513(9) 0.085 Uiso 1 calc R
C15 C 0.6437(16) 0.0493(19) 0.1935(13) 0.101(5) Uani 1 d .
H15A H 0.6849(16) 0.0979(19) 0.1527(13) 0.121 Uiso 1 calc R
C16 C 0.7319(17) -0.0609(23) 0.2567(15) 0.115(7) Uani 1 d .
H16A H 0.8320(17) -0.0847(23) 0.2582(15) 0.137 Uiso 1 calc R
C17 C 0.6726(15) -0.1371(15) 0.3184(11) 0.079(4) Uani 1 d .
H17A H 0.7315(15) -0.2115(15) 0.3600(11) 0.095 Uiso 1 calc R
C18 C 0.5199(12) -0.0957(11) 0.3144(9) 0.060(3) Uani 1 d .
H18A H 0.4773(12) -0.1414(11) 0.3565(9) 0.073 Uiso 1 calc R
C19 C 0.1569(13) 0.1153(10) 0.1386(7) 0.054(3) Uani 1 d .
C20 C 0.2372(23) 0.1125(19) 0.0614(10) 0.108(6) Uani 1 d .
H20A H 0.3372(23) 0.0890(19) 0.0667(10) 0.130 Uiso 1 calc R
C21 C 0.1649(32) 0.1457(21) -0.0240(11) 0.127(8) Uani 1 d .
H21A H 0.2180(32) 0.1442(21) -0.0757(11) 0.152 Uiso 1 calc R
C22 C 0.0212(30) 0.1797(17) -0.0334(13) 0.116(8) Uani 1 d .
H22A H -0.0255(30) 0.2026(17) -0.0908(13) 0.140 Uiso 1 calc R
C23 C -0.0547(24) 0.1802(21) 0.0418(16) 0.134(8) Uani 1 d .
H23A H -0.1538(24) 0.1991(21) 0.0360(16) 0.160 Uiso 1 calc R
C24 C 0.0110(16) 0.1534(15) 0.1273(10) 0.089(5) Uani 1 d .
H24A H -0.0453(16) 0.1616(15) 0.1773(10) 0.106 Uiso 1 calc R
C25 C 0.2030(10) -0.0837(8) 0.2953(6) 0.037(2) Uani 1 d .
C26 C 0.1296(12) -0.1063(10) 0.3713(7) 0.050(3) Uani 1 d .
H26A H 0.1001(12) -0.0488(10) 0.4085(7) 0.060 Uiso 1 calc R
C27 C 0.1003(15) -0.2166(12) 0.3916(9) 0.071(4) Uani 1 d .
H27A H 0.0497(15) -0.2330(12) 0.4425(9) 0.085 Uiso 1 calc R
C28 C 0.1443(16) -0.3007(12) 0.3381(9) 0.073(4) Uani 1 d .
H28A H 0.1246(16) -0.3747(12) 0.3530(9) 0.087 Uiso 1 calc R
C29 C 0.2177(15) -0.2781(11) 0.2623(9) 0.068(3) Uani 1 d .
H29A H 0.2462(15) -0.3353(11) 0.2249(9) 0.082 Uiso 1 calc R
C30 C 0.2480(13) -0.1715(10) 0.2426(8) 0.053(3) Uani 1 d .
H30A H 0.3006(13) -0.1571(10) 0.1923(8) 0.064 Uiso 1 calc R
O2 O 0.5834(14) -0.4369(13) 0.4517(10) 0.128(4) Uiso 1 d .
H2C H 0.5906(14) -0.4551(13) 0.5171(10) 0.153 Uiso 1 d R
H2B H 0.6293(14) -0.5084(13) 0.4248(10) 0.153 Uiso 1 d 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
N2 Re N1 78.2(3) y
N2 Re Cl2 95.1(2) y
N1 Re Cl2 173.2(2) y
N2 Re Cl1 90.2(2) y
N1 Re Cl1 86.0(2) y
Cl2 Re Cl1 94.42(11) y
N2 Re Cl3 170.1(2) y
N1 Re Cl3 92.0(2) y
Cl2 Re Cl3 94.77(11) y
Cl1 Re Cl3 90.53(11) y
N2 Re P 93.7(2) y
N1 Re P 90.7(2) y
Cl2 Re P 89.37(10) y
Cl1 Re P 174.29(9) y
Cl3 Re P 84.89(10) y
C5 N1 C1 119.6(8) ?
C5 N1 Re 114.5(6) y
C1 N1 Re 125.7(7) ?
C6 N2 C7 114.6(7) ?
C6 N2 Re 118.2(6) y
C7 N2 Re 126.6(6) ?
C19 P C13 109.2(5) ?
C19 P C25 99.8(5) ?
C13 P C25 104.3(5) ?
C19 P Re 116.0(4) ?
C13 P Re 108.3(4) ?
C25 P Re 118.3(3) ?
C2 C1 N1 118.1(11) ?
C1 C2 C3 123.9(12) ?
C4 C3 C2 116.3(11) ?
C3 C4 C5 118.9(11) ?
N1 C5 C4 123.1(9) ?
N1 C5 C6 116.3(8) y
C4 C5 C6 120.6(9) ?
O1 C6 N2 127.1(9) y
O1 C6 C5 120.2(9) y
N2 C6 C5 112.7(8) y
C12 C7 C8 117.9(9) ?
C12 C7 N2 121.6(9) ?
C8 C7 N2 120.5(9) ?
C7 C8 C9 120.9(10) ?
C10 C9 C8 119.2(10) ?
C9 C10 C11 121.4(10) ?
C9 C10 Cl4 118.8(9) ?
C11 C10 Cl4 119.8(8) ?
C12 C11 C10 118.1(10) ?
C11 C12 C7 122.4(10) ?
C18 C13 C14 118.9(11) ?
C18 C13 P 120.0(9) ?
C14 C13 P 120.3(9) ?
C15 C14 C13 120.9(14) ?
C14 C15 C16 119.6(16) ?
C15 C16 C17 121.4(14) ?
C16 C17 C18 117.1(14) ?
C13 C18 C17 121.8(14) ?
C24 C19 C20 118.5(13) ?
C24 C19 P 117.7(10) ?
C20 C19 P 123.8(11) ?
C19 C20 C21 118.9(19) ?
C22 C21 C20 121.7(20) ?
C21 C22 C23 118.8(17) ?
C22 C23 C24 121.6(20) ?
C19 C24 C23 120.4(17) ?
C26 C25 C30 119.6(9) ?
C26 C25 P 123.7(8) ?
C30 C25 P 116.6(8) ?
C25 C26 C27 118.5(11) ?
C28 C27 C26 120.7(12) ?
C27 C28 C29 120.7(12) ?
C30 C29 C28 118.9(12) ?
C29 C30 C25 121.5(11) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re N2 2.061(7) y
Re N1 2.123(7) y
Re Cl2 2.300(3) y
Re Cl1 2.331(3) y
Re Cl3 2.345(3) y
Re P 2.549(3) y
N1 C5 1.336(12) y
N1 C1 1.346(13) ?
N2 C6 1.349(12) y
N2 C7 1.436(12) ?
P C19 1.816(11) ?
P C13 1.825(11) ?
P C25 1.841(9) ?
O1 C6 1.217(11) y
Cl4 C10 1.744(10) ?
C1 C2 1.34(2) ?
C2 C3 1.40(2) ?
C3 C4 1.36(2) ?
C4 C5 1.367(14) ?
C5 C6 1.524(13) ?
C7 C12 1.372(14) ?
C7 C8 1.377(14) ?
C8 C9 1.387(15) ?
C9 C10 1.36(2) ?
C10 C11 1.38(2) ?
C11 C12 1.369(15) ?
C13 C18 1.35(2) ?
C13 C14 1.43(2) ?
C14 C15 1.34(2) ?
C15 C16 1.39(3) ?
C16 C17 1.41(3) ?
C17 C18 1.41(2) ?
C19 C24 1.35(2) ?
C19 C20 1.40(2) ?
C20 C21 1.40(2) ?
C21 C22 1.34(3) ?
C22 C23 1.35(3) ?
C23 C24 1.38(2) ?
C25 C26 1.371(14) ?
C25 C30 1.375(13) ?
C26 C27 1.39(2) ?
C27 C28 1.35(2) ?
C28 C29 1.37(2) ?
C29 C30 1.35(2) ?
