#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:33:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179976 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/70/7027052.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_7027052
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 Cl3 N2 P Re'
_chemical_formula_weight         737.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson Heavy Atom'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.66(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.505(6)
_cell_length_b                   13.545(5)
_cell_length_c                   18.720(11)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     2891(3)
_computing_cell_refinement       'Siemens SHELXTL-PLUS P3'
_computing_data_collection       'Siemens SHELXTL-PLUS P3'
_computing_data_reduction        'Siemens SHELXTL-PLUS'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4105
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.558
_exptl_absorpt_correction_T_max  0.3566
_exptl_absorpt_correction_T_min  0.1998
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    'Ridding Model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_obs          0.0316
_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)+(0.0401P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0851
_refine_ls_wR_factor_obs         0.0680
_reflns_number_observed          3065
_reflns_number_total             3801
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806346Jsup1.cif
_cod_data_source_block           fac-ReL1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0401P)^2^+0.0000P] 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^)+(0.0401P)^2^+0.0000P] 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        2891.2(25)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027052
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.14243(2) 0.71607(2) 0.791099(14) 0.02790(11) Uani 1 d .
Cl1 Cl 0.2212(2) 0.61091(14) 0.70565(10) 0.0474(5) Uani 1 d .
Cl2 Cl -0.04667(15) 0.65655(15) 0.75036(10) 0.0456(5) Uani 1 d .
Cl3 Cl 0.1787(2) 0.59209(14) 0.88131(10) 0.0426(5) Uani 1 d .
P1 P 0.0507(2) 0.81950(13) 0.87623(10) 0.0316(4) Uani 1 d .
N1 N 0.3137(4) 0.7715(4) 0.8163(3) 0.0322(14) Uani 1 d .
N2 N 0.1510(5) 0.8306(4) 0.7178(3) 0.0310(13) Uani 1 d .
C1 C 0.3979(6) 0.7358(5) 0.8679(4) 0.041(2) Uani 1 d .
H1 H 0.3795(6) 0.6846(5) 0.8976(4) 0.049 Uiso 1 calc R
C2 C 0.5096(7) 0.7742(6) 0.8769(5) 0.057(2) Uani 1 d .
H2 H 0.5656(7) 0.7486(6) 0.9125(5) 0.068 Uiso 1 calc R
C3 C 0.5395(7) 0.8502(6) 0.8340(5) 0.057(2) Uani 1 d .
H3 H 0.6147(7) 0.8768(6) 0.8410(5) 0.068 Uiso 1 calc R
C4 C 0.4580(6) 0.8853(6) 0.7816(5) 0.051(2) Uani 1 d .
H4 H 0.4769(6) 0.9362(6) 0.7518(5) 0.061 Uiso 1 calc R
C5 C 0.3447(6) 0.8449(5) 0.7720(4) 0.036(2) Uani 1 d .
C6 C 0.2522(6) 0.8755(5) 0.7198(4) 0.039(2) Uani 1 d .
H6 H 0.2626(6) 0.9262(5) 0.6877(4) 0.047 Uiso 1 calc R
C7 C 0.0621(6) 0.8618(5) 0.6617(4) 0.033(2) Uani 1 d .
C8 C 0.0364(6) 0.9610(6) 0.6523(4) 0.043(2) Uani 1 d .
H8 H 0.0748(6) 1.0075(6) 0.6835(4) 0.052 Uiso 1 calc R
C9 C -0.0464(7) 0.9908(7) 0.5962(4) 0.060(2) Uani 1 d .
H9 H -0.0644(7) 1.0575(7) 0.5906(4) 0.072 Uiso 1 calc R
C10 C -0.1021(7) 0.9243(8) 0.5490(4) 0.063(3) Uani 1 d .
H10 H -0.1578(7) 0.9450(8) 0.5114(4) 0.075 Uiso 1 calc R
C11 C -0.0744(8) 0.8251(7) 0.5580(4) 0.061(2) Uani 1 d .
H11 H -0.1115(8) 0.7792(7) 0.5257(4) 0.073 Uiso 1 calc R
C12 C 0.0063(7) 0.7936(6) 0.6134(4) 0.049(2) Uani 1 d .
H12 H 0.0239(7) 0.7267(6) 0.6187(4) 0.059 Uiso 1 calc R
C13 C 0.1607(6) 0.8689(5) 0.9465(4) 0.034(2) Uani 1 d .
C14 C 0.2488(6) 0.9298(5) 0.9271(4) 0.043(2) Uani 1 d .
H14 H 0.2477(6) 0.9471(5) 0.8790(4) 0.051 Uiso 1 calc R
C15 C 0.3373(7) 0.9652(6) 0.9771(5) 0.053(2) Uani 1 d .
H15 H 0.3951(7) 1.0060(6) 0.9629(5) 0.063 Uiso 1 calc R
C16 C 0.3397(7) 0.9394(7) 1.0490(5) 0.061(2) Uani 1 d .
H16 H 0.3994(7) 0.9622(7) 1.0834(5) 0.073 Uiso 1 calc R
C17 C 0.2523(8) 0.8793(7) 1.0688(4) 0.067(3) Uani 1 d .
H17 H 0.2534(8) 0.8618(7) 1.1169(4) 0.080 Uiso 1 calc R
C18 C 0.1633(6) 0.8450(6) 1.0181(4) 0.050(2) Uani 1 d .
H18 H 0.1046(6) 0.8054(6) 1.0324(4) 0.060 Uiso 1 calc R
C19 C -0.0284(6) 0.9254(5) 0.8321(4) 0.036(2) Uani 1 d .
C20 C 0.0081(7) 1.0214(6) 0.8412(4) 0.048(2) Uani 1 d .
H20 H 0.0750(7) 1.0360(6) 0.8731(4) 0.058 Uiso 1 calc R
C21 C -0.0539(8) 1.0974(7) 0.8030(5) 0.065(3) Uani 1 d .
H21 H -0.0268(8) 1.1620(7) 0.8085(5) 0.078 Uiso 1 calc R
C22 C -0.1542(8) 1.0776(8) 0.7576(5) 0.075(3) Uani 1 d .
H22 H -0.1954(8) 1.1284(8) 0.7321(5) 0.090 Uiso 1 calc R
C23 C -0.1946(8) 0.9796(8) 0.7498(5) 0.067(3) Uani 1 d .
H23 H -0.2638(8) 0.9655(8) 0.7200(5) 0.081 Uiso 1 calc R
C24 C -0.1320(6) 0.9053(7) 0.7862(4) 0.053(2) Uani 1 d .
H24 H -0.1585(6) 0.8405(7) 0.7804(4) 0.064 Uiso 1 calc R
C25 C -0.0605(6) 0.7662(5) 0.9276(4) 0.037(2) Uani 1 d .
C26 C -0.0768(7) 0.6661(6) 0.9316(5) 0.057(2) Uani 1 d .
H26 H -0.0365(7) 0.6234(6) 0.9048(5) 0.069 Uiso 1 calc R
C27 C -0.1547(8) 0.6285(7) 0.9764(5) 0.070(3) Uani 1 d .
H27 H -0.1651(8) 0.5606(7) 0.9797(5) 0.084 Uiso 1 calc R
C28 C -0.2151(7) 0.6907(8) 1.0150(5) 0.067(3) Uani 1 d .
H28 H -0.2668(7) 0.6654(8) 1.0445(5) 0.080 Uiso 1 calc R
C29 C -0.1997(7) 0.7909(7) 1.0104(5) 0.063(2) Uani 1 d .
H29 H -0.2411(7) 0.8334(7) 1.0368(5) 0.076 Uiso 1 calc R
C30 C -0.1241(6) 0.8282(6) 0.9674(4) 0.049(2) Uani 1 d .
H30 H -0.1146(6) 0.8962(6) 0.9645(4) 0.058 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'
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 75.9(2) y
N2 Re Cl2 99.5(2) y
N1 Re Cl2 174.1(2) y
N2 Re Cl3 167.0(2) y
N1 Re Cl3 91.3(2) y
Cl2 Re Cl3 93.18(7) y
N2 Re Cl1 87.0(2) y
N1 Re Cl1 86.32(15) y
Cl2 Re Cl1 89.74(7) y
Cl3 Re Cl1 90.46(8) y
N2 Re P1 93.7(2) y
N1 Re P1 96.98(15) y
Cl2 Re P1 86.97(7) y
Cl3 Re P1 89.55(7) y
Cl1 Re P1 176.70(6) y
C13 P1 C19 107.0(3) ?
C13 P1 C25 103.3(3) ?
C19 P1 C25 101.7(3) ?
C13 P1 Re 111.0(2) ?
C19 P1 Re 112.5(2) ?
C25 P1 Re 120.1(2) ?
C1 N1 C5 117.9(6) ?
C1 N1 Re 126.0(5) ?
C5 N1 Re 115.8(4) y
C6 N2 C7 115.5(6) ?
C6 N2 Re 116.6(5) y
C7 N2 Re 127.7(4) ?
N1 C1 C2 121.1(7) ?
C1 C2 C3 120.9(8) ?
C4 C3 C2 118.9(8) ?
C3 C4 C5 119.9(8) ?
N1 C5 C4 121.2(7) ?
N1 C5 C6 113.5(6) y
C4 C5 C6 125.2(7) ?
N2 C6 C5 118.0(6) y
C8 C7 C12 119.5(7) ?
C8 C7 N2 120.0(6) ?
C12 C7 N2 120.3(6) ?
C9 C8 C7 119.7(8) ?
C10 C9 C8 121.2(8) ?
C9 C10 C11 118.8(8) ?
C12 C11 C10 121.2(9) ?
C11 C12 C7 119.6(8) ?
C18 C13 C14 118.1(7) ?
C18 C13 P1 122.6(6) ?
C14 C13 P1 119.2(5) ?
C15 C14 C13 121.9(7) ?
C14 C15 C16 119.3(8) ?
C17 C16 C15 119.2(8) ?
C18 C17 C16 120.8(8) ?
C13 C18 C17 120.6(8) ?
C20 C19 C24 118.9(7) ?
C20 C19 P1 124.1(6) ?
C24 C19 P1 117.0(6) ?
C19 C20 C21 120.7(8) ?
C22 C21 C20 120.4(9) ?
C21 C22 C23 119.3(8) ?
C24 C23 C22 119.9(9) ?
C23 C24 C19 120.8(9) ?
C26 C25 C30 118.7(7) ?
C26 C25 P1 121.6(6) ?
C30 C25 P1 119.5(6) ?
C25 C26 C27 119.7(8) ?
C28 C27 C26 120.3(8) ?
C27 C28 C29 120.0(8) ?
C30 C29 C28 120.1(8) ?
C29 C30 C25 121.1(8) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re N2 2.083(5) y
Re N1 2.103(5) y
Re Cl2 2.350(2) y
Re Cl3 2.379(2) y
Re Cl1 2.407(2) y
Re P1 2.463(2) y
P1 C13 1.827(7) ?
P1 C19 1.835(7) ?
P1 C25 1.846(7) ?
N1 C1 1.363(8) ?
N1 C5 1.371(8) y
N2 C6 1.309(8) y
N2 C7 1.430(8) ?
C1 C2 1.376(10) ?
C2 C3 1.377(11) ?
C3 C4 1.351(10) ?
C4 C5 1.402(9) ?
C5 C6 1.408(9) y
C7 C8 1.382(10) ?
C7 C12 1.389(10) ?
C8 C9 1.380(10) ?
C9 C10 1.361(12) ?
C10 C11 1.386(12) ?
C11 C12 1.365(11) ?
C13 C18 1.375(9) ?
C13 C14 1.392(9) ?
C14 C15 1.374(10) ?
C15 C16 1.387(11) ?
C16 C17 1.382(12) ?
C17 C18 1.381(11) ?
C19 C20 1.370(10) ?
C19 C24 1.400(10) ?
C20 C21 1.394(11) ?
C21 C22 1.365(12) ?
C22 C23 1.408(13) ?
C23 C24 1.366(11) ?
C25 C26 1.373(10) ?
C25 C30 1.393(10) ?
C26 C27 1.402(10) ?
C27 C28 1.359(12) ?
C28 C29 1.373(12) ?
C29 C30 1.359(10) ?
