#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:02:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180023 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/17/7031729.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_7031729
loop_
_publ_author_name
'Chandra Patra, Sarat'
'Saha Roy, Amit'
'Manivannan, Vadivelu'
'Weyhermüller, Thomas'
'Ghosh, Prasanta'
_publ_section_title
;
 Ruthenium, osmium and rhodium complexes of 1,4-diaryl 1,4-diazabutadiene:
 radical versus non-radical states.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13731
_journal_page_last               13741
_journal_paper_doi               10.1039/c4dt01241k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C64 H56 Cl2 N4 O4 P2 Ru'
_chemical_formula_weight         1179.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 114.4320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7677(3)
_cell_length_b                   13.6919(2)
_cell_length_c                   16.3250(2)
_cell_measurement_reflns_used    8613
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      2.38
_cell_volume                     5650.86(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36330
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.234
_diffrn_reflns_theta_min         1.611
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6814
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0289P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4798
_reflns_number_total             6814
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt01241k2.cif
_cod_data_source_block           1.2toluene
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 

 Adding full bibliography for 7031729.cif.
;
_cod_original_cell_volume        5650.85(13)
_cod_database_code               7031729
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.0000 0.13462(2) 0.7500 0.03464(7) Uani 1 2 d S T P . .
P1 P 0.09256(2) 0.11980(3) 0.77997(3) 0.03863(13) Uani 1 1 d . . . . .
Cl1 Cl -0.00965(2) 0.00889(3) 0.64004(3) 0.04738(13) Uani 1 1 d . . . . .
N1 N -0.00837(5) 0.25106(10) 0.66605(10) 0.0378(4) Uani 1 1 d . . . . .
N2 N 0.0300(19) 0.395(3) 0.4231(12) 0.0716(13) Uani 0.586(3) 1 d D . P A 1
O1 O 0.0514(4) 0.4622(10) 0.4742(8) 0.085(2) Uani 0.586(3) 1 d D U P A 1
O2 O 0.0325(5) 0.3825(11) 0.3500(8) 0.111(3) Uani 0.586(3) 1 d D U P A 1
N2' N 0.034(3) 0.400(4) 0.4359(18) 0.0716(13) Uani 0.414(3) 1 d D . P A 2
O1' O 0.0672(7) 0.4509(15) 0.4914(13) 0.085(2) Uani 0.414(3) 1 d D U P A 2
O2' O 0.0194(7) 0.4096(17) 0.3540(13) 0.111(3) Uani 0.414(3) 1 d D U P A 2
C1 C -0.01566(7) 0.25337(13) 0.57368(13) 0.0407(4) Uani 1 1 d . . . . .
C2 C 0.01131(8) 0.32192(14) 0.54601(14) 0.0462(5) Uani 1 1 d . . . . .
H2A H 0.0343 0.3662 0.5867 0.055 Uiso 1 1 calc R U . . .
C3 C 0.00337(8) 0.32276(16) 0.45768(15) 0.0533(5) Uani 1 1 d D . . . .
C4 C -0.02931(9) 0.25712(18) 0.39558(15) 0.0635(6) Uani 1 1 d . . . . .
H4A H -0.0331 0.2580 0.3363 0.076 Uiso 1 1 calc R U . . .
C5 C -0.05617(9) 0.19031(17) 0.42382(15) 0.0601(6) Uani 1 1 d . . . . .
H5A H -0.0790 0.1461 0.3829 0.072 Uiso 1 1 calc R U . . .
C6 C -0.04963(8) 0.18823(14) 0.51194(13) 0.0486(5) Uani 1 1 d . . . . .
H6A H -0.0681 0.1428 0.5302 0.058 Uiso 1 1 calc R U . . .
C7 C -0.00455(8) 0.33714(13) 0.70466(12) 0.0459(5) Uani 1 1 d . . . . .
H7A H -0.0078 0.3950 0.6729 0.069 Uiso 1 1 calc R U . . .
C8 C 0.12275(7) -0.00153(13) 0.78813(13) 0.0426(5) Uani 1 1 d . . . . .
C9 C 0.10156(8) -0.08623(14) 0.80521(13) 0.0494(5) Uani 1 1 d . . . . .
H9A H 0.0694 -0.0840 0.8103 0.059 Uiso 1 1 calc R U . . .
C10 C 0.12765(9) -0.17438(15) 0.81479(14) 0.0582(6) Uani 1 1 d . . . . .
H10A H 0.1133 -0.2306 0.8276 0.070 Uiso 1 1 calc R U . . .
C11 C 0.17415(10) -0.17982(18) 0.80563(15) 0.0689(7) Uani 1 1 d . . . . .
H11A H 0.1913 -0.2395 0.8118 0.083 Uiso 1 1 calc R U . . .
C12 C 0.19531(9) -0.09741(19) 0.78747(17) 0.0757(7) Uani 1 1 d . . . . .
H12A H 0.2267 -0.1010 0.7801 0.091 Uiso 1 1 calc R U . . .
C13 C 0.17035(8) -0.00823(16) 0.77990(16) 0.0623(6) Uani 1 1 d . . . . .
H13A H 0.1857 0.0479 0.7692 0.075 Uiso 1 1 calc R U . . .
C14 C 0.13666(7) 0.17633(14) 0.88602(13) 0.0458(5) Uani 1 1 d . . . . .
C15 C 0.16891(9) 0.11964(17) 0.95849(16) 0.0684(7) Uani 1 1 d . . . . .
H15A H 0.1707 0.0525 0.9516 0.082 Uiso 1 1 calc R U . . .
C16 C 0.19846(11) 0.1623(2) 1.04093(18) 0.0972(10) Uani 1 1 d . . . . .
H16A H 0.2200 0.1236 1.0889 0.117 Uiso 1 1 calc R U . . .
C17 C 0.19637(11) 0.2604(2) 1.05270(19) 0.0984(10) Uani 1 1 d . . . . .
H17A H 0.2163 0.2884 1.1085 0.118 Uiso 1 1 calc R U . . .
C18 C 0.16477(11) 0.31777(19) 0.98207(19) 0.0799(8) Uani 1 1 d . . . . .
H18A H 0.1634 0.3848 0.9899 0.096 Uiso 1 1 calc R U . . .
C19 C 0.13497(8) 0.27638(15) 0.89950(15) 0.0553(6) Uani 1 1 d . . . . .
H19A H 0.1134 0.3159 0.8522 0.066 Uiso 1 1 calc R U . . .
C20 C 0.11088(7) 0.17323(14) 0.69344(13) 0.0426(5) Uani 1 1 d . . . . .
C21 C 0.14457(8) 0.25191(15) 0.70660(15) 0.0587(6) Uani 1 1 d . . . . .
H21A H 0.1584 0.2839 0.7618 0.070 Uiso 1 1 calc R U . . .
C22 C 0.15770(9) 0.28309(18) 0.63747(18) 0.0730(7) Uani 1 1 d . . . . .
H22A H 0.1800 0.3366 0.6467 0.088 Uiso 1 1 calc R U . . .
C23 C 0.13838(9) 0.23632(19) 0.55597(17) 0.0708(7) Uani 1 1 d . . . . .
H23A H 0.1479 0.2573 0.5105 0.085 Uiso 1 1 calc R U . . .
C24 C 0.10507(8) 0.15862(17) 0.54198(15) 0.0603(6) Uani 1 1 d . . . . .
H24A H 0.0918 0.1268 0.4867 0.072 Uiso 1 1 calc R U . . .
C25 C 0.09101(8) 0.12692(14) 0.60950(14) 0.0500(5) Uani 1 1 d . . . . .
H25A H 0.0681 0.0742 0.5990 0.060 Uiso 1 1 calc R U . . .
C31 C 0.1997(2) 0.4347(4) 0.3781(4) 0.0905(15) Uani 0.586(3) 1 d D U P A 1
C32 C 0.1445(2) 0.4473(6) 0.3421(5) 0.0842(18) Uani 0.586(3) 1 d D U P A 1
H32 H 0.1289 0.4470 0.3827 0.101 Uiso 0.586(3) 1 calc R U P A 1
C33 C 0.1142(4) 0.4591(5) 0.2603(5) 0.103(2) Uani 0.586(3) 1 d D U P A 1
H33 H 0.0779 0.4683 0.2407 0.124 Uiso 0.586(3) 1 calc R U P A 1
C34 C 0.1415(3) 0.4569(5) 0.1947(5) 0.117(2) Uani 0.586(3) 1 d D U P A 1
H34 H 0.1220 0.4616 0.1328 0.141 Uiso 0.586(3) 1 calc R U P A 1
C35 C 0.1904(3) 0.4487(5) 0.2274(5) 0.1086(19) Uani 0.586(3) 1 d D U P A 1
H35 H 0.2067 0.4522 0.1878 0.130 Uiso 0.586(3) 1 calc R U P A 1
C36 C 0.2216(3) 0.4352(7) 0.3139(5) 0.0853(18) Uani 0.586(3) 1 d D U P A 1
H36 H 0.2577 0.4260 0.3321 0.102 Uiso 0.586(3) 1 calc R U P A 1
C37 C 0.2317(2) 0.4149(6) 0.4716(5) 0.106(2) Uani 0.586(3) 1 d D U P A 1
H37A H 0.2681 0.4091 0.4811 0.159 Uiso 0.586(3) 1 calc R U P A 1
H37B H 0.2203 0.3549 0.4885 0.159 Uiso 0.586(3) 1 calc R U P A 1
H37C H 0.2281 0.4673 0.5076 0.159 Uiso 0.586(3) 1 calc R U P A 1
C31' C 0.1595(3) 0.4537(5) 0.2933(5) 0.0937(19) Uani 0.414(3) 1 d D U P A 2
C32' C 0.1612(3) 0.4397(9) 0.3809(6) 0.086(2) Uani 0.414(3) 1 d D U P A 2
H32' H 0.1295 0.4436 0.3874 0.104 Uiso 0.414(3) 1 calc R U P A 2
C33' C 0.2029(3) 0.4221(8) 0.4507(8) 0.099(2) Uani 0.414(3) 1 d D U P A 2
H33' H 0.2030 0.4187 0.5077 0.119 Uiso 0.414(3) 1 calc R U P A 2
C34' C 0.2530(3) 0.4071(6) 0.4352(7) 0.092(2) Uani 0.414(3) 1 d D U P A 2
H34' H 0.2844 0.3876 0.4821 0.110 Uiso 0.414(3) 1 calc R U P A 2
C35' C 0.2508(3) 0.4217(6) 0.3575(6) 0.092(2) Uani 0.414(3) 1 d D U P A 2
H35' H 0.2824 0.4176 0.3507 0.110 Uiso 0.414(3) 1 calc R U P A 2
C36' C 0.2079(4) 0.4421(12) 0.2853(7) 0.099(3) Uani 0.414(3) 1 d D U P A 2
H36' H 0.2094 0.4488 0.2297 0.119 Uiso 0.414(3) 1 calc R U P A 2
C37' C 0.1140(4) 0.4748(9) 0.2101(7) 0.118(4) Uani 0.414(3) 1 d D U P A 2
H37D H 0.1250 0.4789 0.1617 0.177 Uiso 0.414(3) 1 calc R U P A 2
H37E H 0.0986 0.5358 0.2158 0.177 Uiso 0.414(3) 1 calc R U P A 2
H37F H 0.0884 0.4236 0.1979 0.177 Uiso 0.414(3) 1 calc R U P A 2
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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 '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_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ru1 N1 78.03(8) . 2_556
N1 Ru1 P1 96.47(4) . 2_556
N1 Ru1 P1 91.02(4) 2_556 2_556
N1 Ru1 P1 91.01(4) . .
N1 Ru1 P1 96.47(4) 2_556 .
P1 Ru1 P1 170.37(2) 2_556 .
N1 Ru1 Cl1 96.32(4) . .
N1 Ru1 Cl1 174.29(4) 2_556 .
P1 Ru1 Cl1 90.449(16) 2_556 .
P1 Ru1 Cl1 82.693(16) . .
N1 Ru1 Cl1 174.29(4) . 2_556
N1 Ru1 Cl1 96.32(4) 2_556 2_556
P1 Ru1 Cl1 82.692(16) 2_556 2_556
P1 Ru1 Cl1 90.451(16) . 2_556
Cl1 Ru1 Cl1 89.34(2) . 2_556
C14 P1 C20 105.62(9) . .
C14 P1 C8 101.95(9) . .
C20 P1 C8 98.75(9) . .
C14 P1 Ru1 113.31(6) . .
C20 P1 Ru1 114.81(6) . .
C8 P1 Ru1 120.30(6) . .
C7 N1 C1 115.48(15) . .
C7 N1 Ru1 114.23(12) . .
C1 N1 Ru1 130.25(11) . .
O1 N2 O2 124.1(9) . .
O1 N2 C3 115.0(14) . .
O2 N2 C3 120.8(16) . .
O1' N2' O2' 123.2(12) . .
O1' N2' C3 124.5(18) . .
O2' N2' C3 112.2(19) . .
C6 C1 C2 119.73(18) . .
C6 C1 N1 120.53(17) . .
C2 C1 N1 119.74(17) . .
C3 C2 C1 118.4(2) . .
C2 C3 C4 122.8(2) . .
C2 C3 N2' 113.6(8) . .
C4 C3 N2' 123.6(8) . .
C2 C3 N2 121.4(6) . .
C4 C3 N2 115.9(6) . .
C5 C4 C3 118.1(2) . .
C6 C5 C4 120.7(2) . .
C5 C6 C1 120.3(2) . .
N1 C7 C7 116.76(10) . 2_556
C9 C8 C13 117.87(18) . .
C9 C8 P1 123.62(15) . .
C13 C8 P1 118.47(15) . .
C8 C9 C10 120.6(2) . .
C11 C10 C9 120.8(2) . .
C12 C11 C10 119.6(2) . .
C11 C12 C13 120.4(2) . .
C12 C13 C8 120.8(2) . .
C15 C14 C19 117.9(2) . .
C15 C14 P1 120.90(16) . .
C19 C14 P1 120.89(16) . .
C16 C15 C14 120.5(2) . .
C17 C16 C15 120.8(3) . .
C16 C17 C18 119.8(3) . .
C17 C18 C19 120.2(2) . .
C18 C19 C14 120.9(2) . .
C21 C20 C25 118.18(19) . .
C21 C20 P1 125.04(16) . .
C25 C20 P1 116.70(14) . .
C20 C21 C22 120.1(2) . .
C23 C22 C21 121.1(2) . .
C24 C23 C22 119.5(2) . .
C23 C24 C25 120.4(2) . .
C24 C25 C20 120.74(19) . .
C32 C31 C36 114.7(6) . .
C32 C31 C37 123.6(6) . .
C36 C31 C37 121.5(6) . .
C33 C32 C31 126.4(7) . .
C32 C33 C34 115.2(8) . .
C35 C34 C33 117.8(7) . .
C34 C35 C36 125.8(8) . .
C35 C36 C31 119.9(6) . .
C36' C31' C32' 116.1(7) . .
C36' C31' C37' 115.4(8) . .
C32' C31' C37' 128.5(9) . .
C33' C32' C31' 124.6(9) . .
C32' C33' C34' 115.7(9) . .
C35' C34' C33' 118.5(8) . .
C34' C35' C36' 125.8(9) . .
C35' C36' C31' 119.1(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.0519(14) .
Ru1 N1 2.0519(14) 2_556
Ru1 P1 2.4179(5) 2_556
Ru1 P1 2.4179(5) .
Ru1 Cl1 2.4206(5) .
Ru1 Cl1 2.4206(5) 2_556
P1 C14 1.828(2) .
P1 C20 1.840(2) .
P1 C8 1.8406(18) .
N1 C7 1.320(2) .
N1 C1 1.437(2) .
N2 O1 1.218(13) .
N2 O2 1.236(17) .
N2 C3 1.480(5) .
N2' O1' 1.216(14) .
N2' O2' 1.235(18) .
N2' C3 1.480(7) .
C1 C6 1.384(3) .
C1 C2 1.388(2) .
C2 C3 1.366(3) .
C3 C4 1.378(3) .
C4 C5 1.375(3) .
C5 C6 1.374(3) .
C7 C7 1.395(4) 2_556
C8 C9 1.380(3) .
C8 C13 1.386(3) .
C9 C10 1.383(3) .
C10 C11 1.362(3) .
C11 C12 1.360(3) .
C12 C13 1.384(3) .
C14 C15 1.388(3) .
C14 C19 1.391(3) .
C15 C16 1.383(3) .
C16 C17 1.361(3) .
C17 C18 1.371(3) .
C18 C19 1.378(3) .
C20 C21 1.384(3) .
C20 C25 1.400(3) .
C21 C22 1.389(3) .
C22 C23 1.370(3) .
C23 C24 1.366(3) .
C24 C25 1.383(3) .
C31 C32 1.408(6) .
C31 C36 1.412(7) .
C31 C37 1.439(8) .
C32 C33 1.260(9) .
C33 C34 1.550(10) .
C34 C35 1.242(7) .
C35 C36 1.329(8) .
C31' C36' 1.412(9) .
C31' C32' 1.424(8) .
C31' C37' 1.451(10) .
C32' C33' 1.267(10) .
C33' C34' 1.526(11) .
C34' C35' 1.261(8) .
C35' C36' 1.313(10) .
