#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/77/7027764.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_7027764
loop_
_publ_author_name
'Chakraborty, Indranil'
'Bhattacharyya, Sibaprasad'
'Banerjee, Sangeeta'
'Kumar Dirghangi, Bimal'
'Chakravorty, Animesh'
_publ_section_title
;
 Synthesis, structure and properties of [ReVL(O)Cl3], [ReVL(NR)Cl3],
 [ReIIIL(OPPh3)Cl3], and [ReIIIL(PPh3)Cl3]
 [L = 2-(arylazo)-1-methylimidazole,
 R = aryl] †
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3747
_journal_paper_doi               10.1039/a906460e
_journal_year                    1999
_chemical_formula_sum            'C28 H24 Cl4 N4 P Re'
_chemical_formula_weight         775.48
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.785(2)
_cell_length_b                   21.183(8)
_cell_length_c                   14.937(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     2927.4(16)
_computing_cell_refinement       'Siemens P3/P4 PC V-4.27'
_computing_data_collection       'Siemens P3/P4 PC V-4.27'
_computing_data_reduction        'Siemens P3/P4 PC V-4.27'
_computing_molecular_graphics    'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_publication_material  'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_structure_refinement  'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'Siemens SHELXTL V-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  '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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5561
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  0.5389
_exptl_absorpt_correction_T_min  0.2194
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.202
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_obs          0.0477
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0635P)²+7.2286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1332
_refine_ls_wR_factor_obs         0.1063
_reflns_number_observed          3719
_reflns_number_total             5138
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906460esup1.cif
_cod_data_source_block           '[ReL3(PPh3)Cl3],5c'
_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^)+(0.0635P)^2^+7.2286P] 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^)+(0.0635P)^2^+7.2286P] 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        2927.3(16)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027764
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 0.70764(4) 0.69885(2) 0.31884(2) 0.02983(14) Uani 1 d .
P1 P 0.7019(3) 0.60547(12) 0.2180(2) 0.0341(6) Uani 1 d .
Cl1 Cl 0.7428(3) 0.78582(13) 0.4269(2) 0.0514(7) Uani 1 d .
Cl2 Cl 0.9508(2) 0.70152(12) 0.3281(2) 0.0427(6) Uani 1 d .
Cl3 Cl 0.7331(3) 0.62931(13) 0.4460(2) 0.0490(7) Uani 1 d .
N1 N 0.4940(9) 0.6976(4) 0.2921(6) 0.042(2) Uani 1 d .
N2 N 0.2757(8) 0.7333(4) 0.2038(6) 0.046(2) Uani 1 d .
N3 N 0.4884(8) 0.7717(4) 0.1728(5) 0.035(2) Uani 1 d .
N4 N 0.6303(8) 0.7610(3) 0.2103(5) 0.032(2) Uani 1 d .
C1 C 0.3875(11) 0.6707(6) 0.3232(9) 0.055(3) Uani 1 d .
H1A H 0.4033(11) 0.6424(6) 0.3732(9) 0.066 Uiso 1 calc R
C2 C 0.2572(12) 0.6928(5) 0.2685(8) 0.054(3) Uani 1 d .
H2A H 0.1686(12) 0.6817(5) 0.2746(8) 0.065 Uiso 1 calc R
C3 C 0.4193(9) 0.7361(4) 0.2182(6) 0.032(2) Uani 1 d .
C4 C 0.1669(12) 0.7704(6) 0.1344(9) 0.065(3) Uani 1 d .
H4A H 0.2120(12) 0.7950(6) 0.0979(9) 0.097 Uiso 1 calc R
H4B H 0.1200(12) 0.7980(6) 0.1663(9) 0.097 Uiso 1 calc R
H4C H 0.0966(12) 0.7427(6) 0.0931(9) 0.097 Uiso 1 calc R
C5 C 0.7084(10) 0.8030(4) 0.1699(6) 0.030(2) Uani 1 d .
C6 C 0.6531(11) 0.8174(4) 0.0737(7) 0.038(2) Uani 1 d .
H6A H 0.5674(11) 0.7991(4) 0.0358(7) 0.046 Uiso 1 calc R
C7 C 0.7282(12) 0.8597(5) 0.0348(8) 0.048(3) Uani 1 d .
H7A H 0.6936(12) 0.8698(5) -0.0292(8) 0.057 Uiso 1 calc R
C8 C 0.8530(11) 0.8858(5) 0.0928(7) 0.039(2) Uani 1 d .
C9 C 0.9062(11) 0.8738(5) 0.1873(7) 0.043(2) Uani 1 d .
H9A H 0.9899(11) 0.8938(5) 0.2248(7) 0.052 Uiso 1 calc R
C10 C 0.8351(10) 0.8317(4) 0.2270(7) 0.035(2) Uani 1 d .
H10A H 0.8712(10) 0.8225(4) 0.2913(7) 0.042 Uiso 1 calc R
C11 C 0.5251(10) 0.5666(5) 0.1771(7) 0.038(2) Uani 1 d .
C12 C 0.4354(13) 0.5615(8) 0.0866(9) 0.080(4) Uani 1 d .
H12A H 0.4645(13) 0.5780(8) 0.0380(9) 0.096 Uiso 1 calc R
C13 C 0.3031(16) 0.5326(10) 0.0644(10) 0.113(7) Uani 1 d .
H13A H 0.2444(16) 0.5298(10) 0.0015(10) 0.135 Uiso 1 calc R
C14 C 0.2567(13) 0.5080(7) 0.1340(11) 0.076(4) Uani 1 d .
H14A H 0.1675(13) 0.4879(7) 0.1189(11) 0.091 Uiso 1 calc R
C15 C 0.3423(13) 0.5131(6) 0.2252(10) 0.065(3) Uani 1 d .
H15A H 0.3113(13) 0.4974(6) 0.2735(10) 0.078 Uiso 1 calc R
C16 C 0.4770(12) 0.5420(6) 0.2467(9) 0.059(3) Uani 1 d .
H16A H 0.5358(12) 0.5448(6) 0.3095(9) 0.070 Uiso 1 calc R
C17 C 0.8227(10) 0.5396(4) 0.2670(7) 0.037(2) Uani 1 d .
C18 C 0.8074(11) 0.4856(5) 0.2127(7) 0.044(2) Uani 1 d .
H18A H 0.7320(11) 0.4827(5) 0.1556(7) 0.052 Uiso 1 calc R
C19 C 0.9031(13) 0.4356(5) 0.2421(9) 0.057(3) Uani 1 d .
H19A H 0.8904(13) 0.3993(5) 0.2052(9) 0.068 Uiso 1 calc R
C20 C 1.0166(13) 0.4394(5) 0.3254(9) 0.062(3) Uani 1 d .
H20A H 1.0825(13) 0.4064(5) 0.3441(9) 0.074 Uiso 1 calc R
C21 C 1.0316(13) 0.4918(5) 0.3801(9) 0.061(3) Uani 1 d .
H21A H 1.1061(13) 0.4940(5) 0.4376(9) 0.074 Uiso 1 calc R
C22 C 0.9360(11) 0.5424(5) 0.3506(8) 0.048(3) Uani 1 d .
H22A H 0.9491(11) 0.5785(5) 0.3880(8) 0.057 Uiso 1 calc R
C23 C 0.7526(10) 0.6262(4) 0.1139(6) 0.036(2) Uani 1 d .
C24 C 0.6595(13) 0.6619(5) 0.0404(7) 0.055(3) Uani 1 d .
H24A H 0.5693(13) 0.6740(5) 0.0428(7) 0.066 Uiso 1 calc R
C25 C 0.7026(16) 0.6793(6) -0.0362(8) 0.071(4) Uani 1 d .
H25A H 0.6395(16) 0.7017(6) -0.0863(8) 0.085 Uiso 1 calc R
C26 C 0.8373(17) 0.6636(6) -0.0381(9) 0.075(4) Uani 1 d .
H26A H 0.8672(17) 0.6765(6) -0.0883(9) 0.090 Uiso 1 calc R
C27 C 0.9277(14) 0.6290(6) 0.0344(8) 0.061(3) Uani 1 d .
H27A H 1.0188(14) 0.6182(6) 0.0323(8) 0.074 Uiso 1 calc R
C28 C 0.8878(10) 0.6096(5) 0.1107(7) 0.043(2) Uani 1 d .
H28A H 0.9506(10) 0.5857(5) 0.1591(7) 0.052 Uiso 1 calc R
Cl4 Cl 0.9453(4) 0.9379(2) 0.0419(2) 0.0699(9) Uani 1 d .
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
N1 Re N4 75.9(3) y
N1 Re Cl2 172.3(2) y
N4 Re Cl2 98.0(2) y
N1 Re Cl3 89.0(2) y
N4 Re Cl3 164.5(2) y
Cl2 Re Cl3 97.41(10) y
N1 Re Cl1 93.2(2) y
N4 Re Cl1 88.5(2) y
Cl2 Re Cl1 91.23(10) y
Cl3 Re Cl1 89.04(10) y
N1 Re P1 93.0(2) y
N4 Re P1 95.9(2) y
Cl2 Re P1 82.92(9) y
Cl3 Re P1 88.07(10) y
Cl1 Re P1 173.08(9) y
C17 P1 C11 102.0(4) ?
C17 P1 C23 101.8(4) ?
C11 P1 C23 108.2(4) ?
C17 P1 Re 119.0(3) ?
C11 P1 Re 113.2(3) ?
C23 P1 Re 111.5(3) ?
C3 N1 C1 104.5(8) ?
C3 N1 Re 113.6(6) y
C1 N1 Re 141.9(7) ?
C2 N2 C3 106.8(8) ?
C2 N2 C4 128.2(9) ?
C3 N2 C4 124.9(9) ?
C3 N3 N4 108.7(7) y
N3 N4 C5 110.1(7) ?
N3 N4 Re 120.6(6) y
C5 N4 Re 129.0(6) ?
C2 C1 N1 108.5(10) ?
N2 C2 C1 109.4(9) ?
N3 C3 N2 128.0(9) ?
N3 C3 N1 121.2(8) y
N2 C3 N1 110.8(8) ?
C6 C5 C10 120.3(8) ?
C6 C5 N4 119.4(8) ?
C10 C5 N4 120.3(8) ?
C5 C6 C7 119.2(9) ?
C8 C7 C6 118.6(10) ?
C9 C8 C7 123.0(9) ?
C9 C8 Cl4 119.5(8) ?
C7 C8 Cl4 117.6(8) ?
C8 C9 C10 119.4(10) ?
C9 C10 C5 119.4(9) ?
C12 C11 C16 117.0(10) ?
C12 C11 P1 127.1(9) ?
C16 C11 P1 115.9(8) ?
C11 C12 C13 122.0(13) ?
C14 C13 C12 120.5(13) ?
C15 C14 C13 119.1(12) ?
C14 C15 C16 119.8(12) ?
C11 C16 C15 121.6(11) ?
C22 C17 C18 118.1(9) ?
C22 C17 P1 123.8(8) ?
C18 C17 P1 117.8(7) ?
C17 C18 C19 120.9(10) ?
C20 C19 C18 120.4(11) ?
C21 C20 C19 119.3(11) ?
C20 C21 C22 120.6(11) ?
C17 C22 C21 120.8(10) ?
C28 C23 C24 119.7(9) ?
C28 C23 P1 119.6(7) ?
C24 C23 P1 120.5(8) ?
C25 C24 C23 119.6(11) ?
C26 C25 C24 120.3(12) ?
C27 C26 C25 119.6(12) ?
C26 C27 C28 121.9(12) ?
C27 C28 C23 118.9(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re N1 1.997(8) y
Re N4 2.035(7) y
Re Cl2 2.338(2) y
Re Cl3 2.352(2) y
Re Cl1 2.399(3) y
Re P1 2.476(3) y
P1 C17 1.822(10) ?
P1 C11 1.831(10) ?
P1 C23 1.833(10) ?
N1 C3 1.376(12) y
N1 C1 1.393(11) ?
N2 C2 1.349(13) ?
N2 C3 1.352(11) y
N2 C4 1.451(13) y
N3 C3 1.335(11) y
N3 N4 1.337(10) y
N4 C5 1.427(11) ?
C1 C2 1.355(15) ?
C5 C6 1.394(12) ?
C5 C10 1.395(13) ?
C6 C7 1.399(13) ?
C7 C8 1.363(14) ?
C8 C9 1.360(13) ?
C8 Cl4 1.748(9) ?
C9 C10 1.379(13) ?
C11 C12 1.356(15) ?
C11 C16 1.375(14) ?
C12 C13 1.37(2) ?
C13 C14 1.37(2) ?
C14 C15 1.35(2) ?
C15 C16 1.393(15) ?
C17 C22 1.376(14) ?
C17 C18 1.382(14) ?
C18 C19 1.386(14) ?
C19 C20 1.37(2) ?
C20 C21 1.36(2) ?
C21 C22 1.396(14) ?
C23 C28 1.384(13) ?
C23 C24 1.399(13) ?
C24 C25 1.39(2) ?
C25 C26 1.37(2) ?
C26 C27 1.37(2) ?
C27 C28 1.383(14) ?
