#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:40:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179983 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/77/7027763.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_7027763
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 O P Re'
_chemical_formula_weight         791.48
_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     'Heavey atom method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.52(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.588(6)
_cell_length_b                   15.007(5)
_cell_length_c                   17.661(8)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     3051(2)
_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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0880
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5194
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.414
_exptl_absorpt_correction_T_max  0.213
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_obs          0.0658
_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)+(0.1059P)²+8.9067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2205
_refine_ls_wR_factor_obs         0.1582
_reflns_number_observed          2611
_reflns_number_total             4774
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906460esup1.cif
_cod_data_source_block           '[ReL3(OPPh3)Cl3],4c'
_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^)+(0.1059P)^2^+8.9067P] 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^)+(0.1059P)^2^+8.9067P] 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        3051.5(23)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027763
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 0.88690(6) 0.74820(6) 0.55420(3) 0.0420(3) Uani 1 d .
Cl1 Cl 0.6972(5) 0.7956(4) 0.5074(3) 0.080(2) Uani 1 d .
Cl2 Cl 0.8855(7) 0.6463(4) 0.4541(3) 0.095(2) Uani 1 d .
Cl3 Cl 0.8792(4) 0.8433(3) 0.6601(3) 0.0567(12) Uani 1 d .
P1 P 0.7590(4) 0.6035(3) 0.6733(3) 0.0460(12) Uani 1 d .
O1 O 0.8279(10) 0.6472(8) 0.6168(7) 0.049(3) Uani 1 d .
N1 N 0.9608(13) 0.8403(10) 0.4936(8) 0.049(4) Uani 1 d .
N3 N 1.1371(14) 0.7882(10) 0.5602(8) 0.050(4) Uani 1 d .
N4 N 1.0557(13) 0.7328(10) 0.5828(10) 0.057(4) Uani 1 d .
N2 N 1.1187(17) 0.9083(11) 0.4667(9) 0.065(5) Uani 1 d .
C1 C 0.9320(18) 0.9037(13) 0.4395(9) 0.055(5) Uani 1 d .
H1A H 0.8570(18) 0.9179(13) 0.4185(9) 0.066 Uiso 1 calc R
C2 C 1.0289(21) 0.9420(14) 0.4216(11) 0.066(6) Uani 1 d .
H2A H 1.0333(21) 0.9848(14) 0.3840(11) 0.080 Uiso 1 calc R
C3 C 1.0769(19) 0.8444(12) 0.5111(11) 0.058(5) Uani 1 d .
C4 C 1.2406(21) 0.9329(17) 0.4681(16) 0.102(9) Uani 1 d .
H4A H 1.2865(21) 0.8982(17) 0.5061(16) 0.153 Uiso 1 calc R
H4B H 1.2498(21) 0.9951(17) 0.4802(16) 0.153 Uiso 1 calc R
H4C H 1.2658(21) 0.9218(17) 0.4191(16) 0.153 Uiso 1 calc R
C5 C 1.1073(16) 0.6678(12) 0.6367(11) 0.052(5) Uani 1 d .
C6 C 1.0836(20) 0.5804(13) 0.6250(11) 0.068(6) Uani 1 d .
H6A H 1.0321(20) 0.5617(13) 0.5839(11) 0.081 Uiso 1 calc R
C7 C 1.1379(21) 0.5196(14) 0.6758(13) 0.072(6) Uani 1 d .
H7A H 1.1180(21) 0.4598(14) 0.6700(13) 0.087 Uiso 1 calc R
C8 C 1.2184(18) 0.5433(13) 0.7334(13) 0.066(6) Uani 1 d .
C9 C 1.2385(21) 0.6340(15) 0.7479(13) 0.081(7) Uani 1 d .
H9A H 1.2874(21) 0.6525(15) 0.7904(13) 0.097 Uiso 1 calc R
C10 C 1.1846(16) 0.6945(13) 0.6984(11) 0.057(5) Uani 1 d .
H10A H 1.2000(16) 0.7548(13) 0.7060(11) 0.068 Uiso 1 calc R
C11 C 0.6916(19) 0.5047(13) 0.6306(10) 0.063(6) Uani 1 d .
C12 C 0.5939(21) 0.4669(16) 0.6577(13) 0.084(8) Uani 1 d .
H12A H 0.5621(21) 0.4929(16) 0.6984(13) 0.101 Uiso 1 calc R
C13 C 0.5450(26) 0.3915(21) 0.6243(16) 0.117(12) Uani 1 d .
H13A H 0.4811(26) 0.3657(21) 0.6430(16) 0.141 Uiso 1 calc R
C14 C 0.5896(35) 0.3544(21) 0.5637(20) 0.135(13) Uani 1 d .
H14A H 0.5537(35) 0.3054(21) 0.5388(20) 0.162 Uiso 1 calc R
C15 C 0.6913(32) 0.3914(21) 0.5393(16) 0.134(13) Uani 1 d .
H15A H 0.7284(32) 0.3625(21) 0.5023(16) 0.160 Uiso 1 calc R
C16 C 0.7342(23) 0.4677(15) 0.5693(12) 0.092(9) Uani 1 d .
H16A H 0.7942(23) 0.4959(15) 0.5480(12) 0.110 Uiso 1 calc R
C17 C 0.8540(15) 0.5734(12) 0.7558(10) 0.048(5) Uani 1 d .
C18 C 0.8533(18) 0.4921(13) 0.7905(12) 0.062(5) Uani 1 d .
H18A H 0.8001(18) 0.4490(13) 0.7713(12) 0.074 Uiso 1 calc R
C19 C 0.9317(22) 0.4730(17) 0.8546(13) 0.078(8) Uani 1 d .
H19A H 0.9350(22) 0.4167(17) 0.8767(13) 0.094 Uiso 1 calc R
C20 C 1.0036(23) 0.5402(22) 0.8838(14) 0.094(9) Uani 1 d .
H20A H 1.0541(23) 0.5288(22) 0.9274(14) 0.113 Uiso 1 calc R
C21 C 1.0047(18) 0.6209(16) 0.8528(12) 0.067(6) Uani 1 d .
H21A H 1.0548(18) 0.6653(16) 0.8733(12) 0.081 Uiso 1 calc R
C22 C 0.9267(18) 0.6354(14) 0.7878(10) 0.063(6) Uani 1 d .
H22A H 0.9253(18) 0.6915(14) 0.7654(10) 0.075 Uiso 1 calc R
C23 C 0.6465(16) 0.6750(14) 0.7026(10) 0.057(5) Uani 1 d .
C24 C 0.5529(18) 0.6944(16) 0.6501(12) 0.068(6) Uani 1 d .
H24A H 0.5489(18) 0.6708(16) 0.6012(12) 0.082 Uiso 1 calc R
C25 C 0.4655(19) 0.7482(19) 0.6697(17) 0.091(8) Uani 1 d .
H25A H 0.4029(19) 0.7625(19) 0.6341(17) 0.109 Uiso 1 calc R
C26 C 0.4716(23) 0.7796(18) 0.7401(20) 0.096(9) Uani 1 d .
H26A H 0.4112(23) 0.8148(18) 0.7537(20) 0.115 Uiso 1 calc R
C27 C 0.5608(23) 0.7626(18) 0.7920(16) 0.091(8) Uani 1 d .
H27A H 0.5632(23) 0.7874(18) 0.8404(16) 0.110 Uiso 1 calc R
C28 C 0.6507(18) 0.7078(15) 0.7743(12) 0.066(6) Uani 1 d .
H28A H 0.7124(18) 0.6940(15) 0.8109(12) 0.079 Uiso 1 calc R
Cl4 Cl 1.2837(7) 0.4643(4) 0.7947(4) 0.102(2) 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'
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 75.3(6) y
N4 Re O1 99.0(6) y
N1 Re O1 173.9(5) y
N4 Re Cl2 92.2(5) y
N1 Re Cl2 90.8(5) y
O1 Re Cl2 87.1(4) y
N4 Re Cl3 89.7(4) y
N1 Re Cl3 93.6(4) y
O1 Re Cl3 88.6(4) y
Cl2 Re Cl3 175.5(2) y
N4 Re Cl1 167.5(5) y
N1 Re Cl1 92.4(5) y
O1 Re Cl1 93.3(4) y
Cl2 Re Cl1 90.4(3) y
Cl3 Re Cl1 88.7(2) y
O1 P1 C17 109.2(8) ?
O1 P1 C11 108.7(8) ?
C17 P1 C11 109.4(9) ?
O1 P1 C23 112.8(8) ?
C17 P1 C23 108.3(8) ?
C11 P1 C23 108.4(10) ?
P1 O1 Re 157.4(8) y
C3 N1 C1 106.6(16) ?
C3 N1 Re 112.8(12) y
C1 N1 Re 140.6(14) ?
C3 N3 N4 104.4(15) y
N3 N4 C5 111.1(15) ?
N3 N4 Re 123.7(13) y
C5 N4 Re 124.8(12) ?
C2 N2 C3 107.8(18) ?
C2 N2 C4 127.0(19) ?
C3 N2 C4 125.2(21) ?
C2 C1 N1 108.8(18) ?
C1 C2 N2 108.4(19) ?
N1 C3 N3 123.3(16) y
N1 C3 N2 108.2(19) ?
N3 C3 N2 128.3(20) ?
C6 C5 C10 120.1(18) ?
C6 C5 N4 119.5(19) ?
C10 C5 N4 120.4(17) ?
C5 C6 C7 118.2(20) ?
C8 C7 C6 122.8(20) ?
C7 C8 C9 118.7(21) ?
C7 C8 Cl4 120.7(16) ?
C9 C8 Cl4 120.2(18) ?
C10 C9 C8 118.4(20) ?
C9 C10 C5 121.3(18) ?
C16 C11 C12 119.2(19) ?
C16 C11 P1 119.4(16) ?
C12 C11 P1 121.4(17) ?
C13 C12 C11 119.9(25) ?
C14 C13 C12 120.2(25) ?
C13 C14 C15 118.9(27) ?
C16 C15 C14 120.1(30) ?
C15 C16 C11 121.0(24) ?
C22 C17 C18 117.9(19) ?
C22 C17 P1 118.1(15) ?
C18 C17 P1 124.0(16) ?
C17 C18 C19 120.6(21) ?
C20 C19 C18 117.7(21) ?
C21 C20 C19 123.3(22) ?
C20 C21 C22 116.4(22) ?
C17 C22 C21 123.9(20) ?
C28 C23 C24 119.7(20) ?
C28 C23 P1 122.2(16) ?
C24 C23 P1 118.1(15) ?
C25 C24 C23 120.3(22) ?
C26 C25 C24 118.9(25) ?
C25 C26 C27 122.4(25) ?
C26 C27 C28 120.2(24) ?
C23 C28 C27 118.5(21) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Re N4 1.978(15) y
Re N1 1.999(14) y
Re O1 2.039(11) y
Re Cl2 2.336(6) y
Re Cl3 2.363(5) y
Re Cl1 2.369(6) y
P1 O1 1.498(12) y
P1 C17 1.78(2) ?
P1 C11 1.80(2) ?
P1 C23 1.81(2) ?
N1 C3 1.35(2) y
N1 C1 1.36(2) ?
N3 C3 1.35(2) y
N3 N4 1.351(20) y
N4 C5 1.44(2) ?
N2 C2 1.34(3) ?
N2 C3 1.36(2) ?
N2 C4 1.46(3) ?
C1 C2 1.33(3) ?
C5 C6 1.35(2) ?
C5 C10 1.39(2) ?
C6 C7 1.38(3) ?
C7 C8 1.35(3) ?
C8 C9 1.40(3) ?
C8 Cl4 1.72(2) ?
C9 C10 1.36(3) ?
C11 C16 1.36(3) ?
C11 C12 1.40(3) ?
C12 C13 1.37(3) ?
C13 C14 1.36(4) ?
C14 C15 1.41(4) ?
C15 C16 1.33(3) ?
C17 C22 1.34(2) ?
C17 C18 1.37(3) ?
C18 C19 1.40(3) ?
C19 C20 1.37(3) ?
C20 C21 1.33(3) ?
C21 C22 1.40(3) ?
C23 C28 1.35(3) ?
C23 C24 1.38(3) ?
C24 C25 1.37(3) ?
C25 C26 1.32(4) ?
C26 C27 1.33(4) ?
C27 C28 1.39(3) ?
