#------------------------------------------------------------------------------
#$Date: 2019-12-26 20:47:32 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/16/2311672.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2311672
loop_
_publ_author_name
'Kumar, Sandeep'
'Khajuria, Ruchi'
'Jassal, Amanpreet Kaur'
'Hundal, Maninder S.'
'Pandey, Sushil K.'
_publ_section_title
;
 Synthesis and structural elucidation of new complexes of 2,4- and
 3,5-dimethyl diphenyldithiophosphates with cobalt(II).
;
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              221
_journal_page_last               227
_journal_paper_doi               10.1107/S205252061500390X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'C46 H54 Co N2 O4 P2 S4'
_chemical_formula_sum            'C46 H54 Co N2 O4 P2 S4'
_chemical_formula_weight         948.06
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.290(3)
_cell_angle_beta                 98.602(3)
_cell_angle_gamma                112.994(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5631(7)
_cell_length_b                   9.8309(6)
_cell_length_c                   14.2326(9)
_cell_measurement_reflns_used    5679
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.32
_cell_volume                     1181.83(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24294
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             497
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0397P)²+0.2495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                3991
_reflns_number_total             5258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5076sup1.cif
_cod_data_source_block           35_Co_ETPY_0m
_cod_database_code               2311672
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.2565(2) 0.9175(2) 0.93807(15) 0.0375(5) Uani d . 1 1
H H1 0.3101 1.0230 0.9522 0.045 Uiso calc R 1 1
C C2 0.3336(3) 0.8316(2) 0.90884(15) 0.0396(5) Uani d . 1 1
H H2 0.4367 0.8793 0.9042 0.047 Uiso calc R 1 1
C C3 0.2575(3) 0.6743(2) 0.88627(16) 0.0417(5) Uani d . 1 1
C C4 0.1039(3) 0.6124(2) 0.89462(18) 0.0485(6) Uani d . 1 1
H H4 0.0473 0.5072 0.8800 0.058 Uiso calc R 1 1
C C5 0.0351(3) 0.7056(2) 0.92433(17) 0.0435(5) Uani d . 1 1
H H5 -0.0684 0.6606 0.9288 0.052 Uiso calc R 1 1
C C6 0.3373(3) 0.5747(3) 0.8552(2) 0.0582(7) Uani d . 1 1
H H6A 0.4473 0.6387 0.8626 0.070 Uiso calc R 1 1
H H6B 0.3297 0.5066 0.8984 0.070 Uiso calc R 1 1
C C7 0.2692(4) 0.4818(3) 0.7514(2) 0.0730(9) Uani d . 1 1
H H7A 0.1604 0.4180 0.7434 0.110 Uiso calc R 1 1
H H7B 0.3230 0.4195 0.7365 0.110 Uiso calc R 1 1
H H7C 0.2807 0.5485 0.7079 0.110 Uiso calc R 1 1
C C8 -0.2096(3) 1.1765(2) 0.72296(16) 0.0413(5) Uani d . 1 1
C C9 -0.1775(3) 1.2691(2) 0.65879(17) 0.0486(6) Uani d . 1 1
H H9 -0.1249 1.2534 0.6112 0.058 Uiso calc R 1 1
C C10 -0.2249(3) 1.3868(3) 0.6662(2) 0.0587(7) Uani d . 1 1
C C11 -0.3055(3) 1.4047(3) 0.7367(2) 0.0632(8) Uani d . 1 1
H H11 -0.3369 1.4835 0.7421 0.076 Uiso calc R 1 1
C C12 -0.3407(3) 1.3093(3) 0.79913(19) 0.0599(7) Uani d . 1 1
C C13 -0.2894(3) 1.1949(3) 0.79320(18) 0.0510(6) Uani d . 1 1
H H13 -0.3088 1.1314 0.8362 0.061 Uiso calc R 1 1
C C14 -0.4379(5) 1.3260(5) 0.8709(2) 0.1085(14) Uani d . 1 1
H H14A -0.4136 1.4317 0.8941 0.163 Uiso calc R 1 1
H H14B -0.4150 1.2855 0.9253 0.163 Uiso calc R 1 1
H H14C -0.5467 1.2712 0.8390 0.163 Uiso calc R 1 1
C C15 -0.1878(5) 1.4939(3) 0.5980(3) 0.0972(12) Uani d . 1 1
H H15A -0.2813 1.4706 0.5503 0.146 Uiso calc R 1 1
H H15B -0.1112 1.4813 0.5654 0.146 Uiso calc R 1 1
H H15C -0.1475 1.5972 0.6354 0.146 Uiso calc R 1 1
C C16 0.0980(3) 0.9486(2) 0.67280(14) 0.0369(5) Uani d . 1 1
C C17 0.1929(3) 0.8739(2) 0.67599(15) 0.0401(5) Uani d . 1 1
H H17 0.1725 0.7942 0.7071 0.048 Uiso calc R 1 1
C C18 0.3195(3) 0.9173(3) 0.63267(16) 0.0455(5) Uani d . 1 1
C C19 0.3460(3) 1.0362(3) 0.58696(16) 0.0476(6) Uani d . 1 1
H H19 0.4315 1.0673 0.5588 0.057 Uiso calc R 1 1
C C20 0.2492(3) 1.1099(2) 0.58185(15) 0.0445(5) Uani d . 1 1
C C21 0.1234(3) 1.0646(2) 0.62509(16) 0.0442(5) Uani d . 1 1
H H21 0.0562 1.1122 0.6220 0.053 Uiso calc R 1 1
C C22 0.4261(3) 0.8373(3) 0.6363(2) 0.0663(7) Uani d . 1 1
H H22A 0.5131 0.8888 0.6096 0.099 Uiso calc R 1 1
H H22B 0.3693 0.7338 0.5986 0.099 Uiso calc R 1 1
H H22C 0.4634 0.8383 0.7030 0.099 Uiso calc R 1 1
C C23 0.2787(4) 1.2362(3) 0.52887(19) 0.0626(7) Uani d . 1 1
H H23A 0.2002 1.2736 0.5320 0.094 Uiso calc R 1 1
H H23B 0.2749 1.1977 0.4616 0.094 Uiso calc R 1 1
H H23C 0.3799 1.3175 0.5593 0.094 Uiso calc R 1 1
N N1 0.1091(2) 0.85802(18) 0.94729(12) 0.0349(4) Uani d . 1 1
S S1 -0.09726(6) 0.83156(6) 1.11663(4) 0.03892(14) Uani d . 1 1
S S2 -0.22936(6) 0.86021(6) 0.85104(4) 0.03851(14) Uani d . 1 1
O O1 -0.16621(18) 1.05524(16) 0.70770(10) 0.0432(4) Uani d . 1 1
O O2 -0.02978(18) 0.89432(15) 0.71634(10) 0.0408(4) Uani d . 1 1
P P1 -0.08148(6) 0.99841(6) 0.78859(4) 0.03383(14) Uani d . 1 1
Co Co1 0.0000 1.0000 1.0000 0.03154(11) Uani d S 1 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 C2 . . 123.73(19)
N1 C1 H1 . . 118.1
C2 C1 H1 . . 118.1
C1 C2 C3 . . 120.0(2)
C1 C2 H2 . . 120.0
C3 C2 H2 . . 120.0
C2 C3 C4 . . 116.34(19)
C2 C3 C6 . . 122.1(2)
C4 C3 C6 . . 121.53(19)
C5 C4 C3 . . 120.28(19)
C5 C4 H4 . . 119.9
C3 C4 H4 . . 119.9
N1 C5 C4 . . 123.5(2)
N1 C5 H5 . . 118.3
C4 C5 H5 . . 118.3
C7 C6 C3 . . 113.4(2)
C7 C6 H6A . . 108.9
C3 C6 H6A . . 108.9
C7 C6 H6B . . 108.9
C3 C6 H6B . . 108.9
H6A C6 H6B . . 107.7
C6 C7 H7A . . 109.5
C6 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
C6 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
C9 C8 C13 . . 122.0(2)
C9 C8 O1 . . 115.8(2)
C13 C8 O1 . . 122.0(2)
C8 C9 C10 . . 119.0(2)
C8 C9 H9 . . 120.5
C10 C9 H9 . . 120.5
C11 C10 C9 . . 118.8(2)
C11 C10 C15 . . 120.8(3)
C9 C10 C15 . . 120.4(3)
C12 C11 C10 . . 121.9(2)
C12 C11 H11 . . 119.0
C10 C11 H11 . . 119.0
C11 C12 C13 . . 119.0(3)
C11 C12 C14 . . 120.5(2)
C13 C12 C14 . . 120.5(3)
C8 C13 C12 . . 119.2(2)
C8 C13 H13 . . 120.4
C12 C13 H13 . . 120.4
C12 C14 H14A . . 109.5
C12 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C12 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
C10 C15 H15A . . 109.5
C10 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C10 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
C17 C16 C21 . . 121.2(2)
C17 C16 O2 . . 116.03(18)
C21 C16 O2 . . 122.65(19)
C16 C17 C18 . . 119.9(2)
C16 C17 H17 . . 120.0
C18 C17 H17 . . 120.0
C19 C18 C17 . . 118.3(2)
C19 C18 C22 . . 121.0(2)
C17 C18 C22 . . 120.6(2)
C20 C19 C18 . . 122.0(2)
C20 C19 H19 . . 119.0
C18 C19 H19 . . 119.0
C19 C20 C21 . . 118.8(2)
C19 C20 C23 . . 120.6(2)
C21 C20 C23 . . 120.5(2)
C16 C21 C20 . . 119.6(2)
C16 C21 H21 . . 120.2
C20 C21 H21 . . 120.2
C18 C22 H22A . . 109.5
C18 C22 H22B . . 109.5
H22A C22 H22B . . 109.5
C18 C22 H22C . . 109.5
H22A C22 H22C . . 109.5
H22B C22 H22C . . 109.5
C20 C23 H23A . . 109.5
C20 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C20 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
C1 N1 C5 . . 116.18(17)
C1 N1 Co1 . . 121.54(13)
C5 N1 Co1 . . 122.26(14)
P1 S1 Co1 2_577 . 81.66(2)
P1 S2 Co1 . . 81.59(2)
C8 O1 P1 . . 127.68(13)
C16 O2 P1 . . 125.27(12)
O2 P1 O1 . . 98.00(8)
O2 P1 S1 . 2_577 112.95(6)
O1 P1 S1 . 2_577 112.31(6)
O2 P1 S2 . . 106.33(6)
O1 P1 S2 . . 112.76(7)
S1 P1 S2 2_577 . 113.37(4)
N1 Co1 N1 2_577 . 179.9990(10)
N1 Co1 S2 2_577 . 90.26(5)
N1 Co1 S2 . . 89.74(5)
N1 Co1 S2 2_577 2_577 89.74(5)
N1 Co1 S2 . 2_577 90.26(5)
S2 Co1 S2 . 2_577 180.0
N1 Co1 S1 2_577 2_577 89.23(5)
N1 Co1 S1 . 2_577 90.77(5)
S2 Co1 S1 . 2_577 80.532(18)
S2 Co1 S1 2_577 2_577 99.467(18)
N1 Co1 S1 2_577 . 90.77(5)
N1 Co1 S1 . . 89.23(5)
S2 Co1 S1 . . 99.468(19)
S2 Co1 S1 2_577 . 80.533(18)
S1 Co1 S1 2_577 . 179.9990(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.335(3)
C1 C2 . 1.376(3)
C1 H1 . 0.9300
C2 C3 . 1.384(3)
C2 H2 . 0.9300
C3 C4 . 1.385(3)
C3 C6 . 1.510(3)
C4 C5 . 1.372(3)
C4 H4 . 0.9300
C5 N1 . 1.341(2)
C5 H5 . 0.9300
C6 C7 . 1.501(4)
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 H7A . 0.9600
C7 H7B . 0.9600
C7 H7C . 0.9600
C8 C9 . 1.375(3)
C8 C13 . 1.376(3)
C8 O1 . 1.404(2)
C9 C10 . 1.393(3)
C9 H9 . 0.9300
C10 C11 . 1.383(4)
C10 C15 . 1.521(4)
C11 C12 . 1.376(4)
C11 H11 . 0.9300
C12 C13 . 1.388(3)
C12 C14 . 1.511(4)
C13 H13 . 0.9300
C14 H14A . 0.9600
C14 H14B . 0.9600
C14 H14C . 0.9600
C15 H15A . 0.9600
C15 H15B . 0.9600
C15 H15C . 0.9600
C16 C17 . 1.372(3)
C16 C21 . 1.380(3)
C16 O2 . 1.409(2)
C17 C18 . 1.391(3)
C17 H17 . 0.9300
C18 C19 . 1.384(3)
C18 C22 . 1.511(3)
C19 C20 . 1.381(3)
C19 H19 . 0.9300
C20 C21 . 1.384(3)
C20 C23 . 1.511(3)
C21 H21 . 0.9300
C22 H22A . 0.9600
C22 H22B . 0.9600
C22 H22C . 0.9600
C23 H23A . 0.9600
C23 H23B . 0.9600
C23 H23C . 0.9600
N1 Co1 . 2.1523(16)
S1 P1 2_577 1.9712(8)
S1 Co1 . 2.5512(5)
S2 P1 . 1.9750(8)
S2 Co1 . 2.5510(6)
O1 P1 . 1.6051(15)
O2 P1 . 1.5989(14)
P1 S1 2_577 1.9712(8)
Co1 N1 2_577 2.1523(16)
Co1 S2 2_577 2.5510(6)
Co1 S1 2_577 2.5512(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 C1 C2 C3 . . 0.6(3)
C1 C2 C3 C4 . . 0.3(3)
C1 C2 C3 C6 . . -179.1(2)
C2 C3 C4 C5 . . -0.3(3)
C6 C3 C4 C5 . . 179.1(2)
C3 C4 C5 N1 . . -0.4(4)
C2 C3 C6 C7 . . -114.2(3)
C4 C3 C6 C7 . . 66.5(3)
C13 C8 C9 C10 . . 1.1(4)
O1 C8 C9 C10 . . 176.57(19)
C8 C9 C10 C11 . . -1.3(4)
C8 C9 C10 C15 . . 178.5(2)
C9 C10 C11 C12 . . -0.3(4)
C15 C10 C11 C12 . . 179.9(3)
C10 C11 C12 C13 . . 2.1(4)
C10 C11 C12 C14 . . -176.1(3)
C9 C8 C13 C12 . . 0.7(4)
O1 C8 C13 C12 . . -174.5(2)
C11 C12 C13 C8 . . -2.2(4)
C14 C12 C13 C8 . . 175.9(3)
C21 C16 C17 C18 . . 1.6(3)
O2 C16 C17 C18 . . 178.40(18)
C16 C17 C18 C19 . . -0.1(3)
C16 C17 C18 C22 . . 179.4(2)
C17 C18 C19 C20 . . -1.2(3)
C22 C18 C19 C20 . . 179.3(2)
C18 C19 C20 C21 . . 1.0(3)
C18 C19 C20 C23 . . -178.2(2)
C17 C16 C21 C20 . . -1.8(3)
O2 C16 C21 C20 . . -178.43(18)
C19 C20 C21 C16 . . 0.6(3)
C23 C20 C21 C16 . . 179.7(2)
C2 C1 N1 C5 . . -1.3(3)
C2 C1 N1 Co1 . . 177.05(16)
C4 C5 N1 C1 . . 1.2(3)
C4 C5 N1 Co1 . . -177.11(18)
C9 C8 O1 P1 . . 136.37(18)
C13 C8 O1 P1 . . -48.2(3)
C17 C16 O2 P1 . . 134.26(16)
C21 C16 O2 P1 . . -49.0(3)
C16 O2 P1 O1 . . 77.52(17)
C16 O2 P1 S1 . 2_577 -40.90(17)
C16 O2 P1 S2 . . -165.85(14)
C8 O1 P1 O2 . . -165.06(17)
C8 O1 P1 S1 . 2_577 -46.16(19)
C8 O1 P1 S2 . . 83.42(18)
Co1 S2 P1 O2 . . 109.61(6)
Co1 S2 P1 O1 . . -144.12(6)
Co1 S2 P1 S1 . 2_577 -15.09(3)
C1 N1 Co1 S2 . . 128.14(16)
C5 N1 Co1 S2 . . -53.64(16)
C1 N1 Co1 S2 . 2_577 -51.86(16)
C5 N1 Co1 S2 . 2_577 126.36(16)
C1 N1 Co1 S1 . 2_577 47.61(16)
C5 N1 Co1 S1 . 2_577 -134.16(16)
C1 N1 Co1 S1 . . -132.39(16)
C5 N1 Co1 S1 . . 45.84(16)
P1 S2 Co1 N1 . 2_577 99.96(5)
P1 S2 Co1 N1 . . -80.04(5)
P1 S2 Co1 S1 . 2_577 10.79(2)
P1 S2 Co1 S1 . . -169.21(2)
P1 S1 Co1 N1 2_577 2_577 -78.80(5)
P1 S1 Co1 N1 2_577 . 101.20(5)
P1 S1 Co1 S2 2_577 . -169.19(2)
P1 S1 Co1 S2 2_577 2_577 10.81(2)
