#------------------------------------------------------------------------------
#$Date: 2017-04-05 13:12:45 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195192 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/53/1545300.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_1545300
loop_
_publ_author_name
'Chen, Huafeng'
'Pan, Weijing'
'Huang, Kuo-Wei'
'Zhang, Xuequan'
'Gong, Dirong'
_publ_section_title
;
 Controlled polymerization of isoprene promoted by a type of hemilabile
 XPN3 (X = O, S) ligand supported cobalt(ii) complexes: the role
 of a hemilabile donor on the level of control
;
_journal_issue                   11
_journal_name_full               'Polym. Chem.'
_journal_page_first              1805
_journal_paper_doi               10.1039/C7PY00252A
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C44 H42 Cl4 Co2 N8 P2 S2'
_chemical_formula_sum            'C44 H42 Cl4 Co2 N8 P2 S2'
_chemical_formula_weight         1068.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-11-23 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.147(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4650(10)
_cell_length_b                   15.7090(16)
_cell_length_c                   16.2919(16)
_cell_measurement_reflns_used    2694
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.148
_cell_measurement_theta_min      2.593
_cell_volume                     2326.8(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13806
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         2.588
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0412
_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)+(0.0414P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3738
_reflns_number_total             5257
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7py00252a2.cif
_cod_data_source_block           gdr47_0m
_cod_depositor_comments
'Adding full bibliography for 1545298--1545301.cif.'
_cod_database_code               1545300
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Co1 Co 0.14783(4) 0.47572(2) 0.59144(2) 0.01536(11) Uani 1 1 d .
Cl2 Cl 0.08100(7) 0.44015(5) 0.44605(5) 0.02207(17) Uani 1 1 d .
Cl1 Cl 0.08088(9) 0.37933(5) 0.67709(6) 0.0342(2) Uani 1 1 d .
S3 S 0.46103(9) 0.11211(5) 0.64003(5) 0.0298(2) Uani 1 1 d .
P1 P 0.29310(8) 0.16842(5) 0.56394(5) 0.01732(17) Uani 1 1 d .
N1 N 0.2981(2) 0.57009(15) 0.63537(14) 0.0173(5) Uani 1 1 d .
N2 N 0.4425(2) 0.54850(14) 0.64332(14) 0.0158(5) Uani 1 1 d .
N3 N 0.3646(2) 0.41184(14) 0.60356(14) 0.0143(5) Uani 1 1 d .
N4 N 0.2791(2) 0.27409(14) 0.57798(15) 0.0188(5) Uani 1 1 d .
H4 H 0.1969 0.2932 0.5866 0.023 Uiso 1 1 d R
C1 C 0.4722(3) 0.46915(17) 0.61069(17) 0.0158(6) Uani 1 1 d .
C2 C 0.3877(3) 0.33311(17) 0.57713(17) 0.0158(6) Uani 1 1 d .
C3 C 0.2924(3) 0.15861(17) 0.45307(18) 0.0176(6) Uani 1 1 d .
C4 C 0.3987(3) 0.11035(18) 0.4301(2) 0.0228(7) Uani 1 1 d .
H4A H 0.4713 0.0808 0.4726 0.027 Uiso 1 1 calc R
C5 C 0.3989(3) 0.10532(19) 0.3451(2) 0.0287(7) Uani 1 1 d .
H5 H 0.4733 0.0737 0.3298 0.034 Uiso 1 1 calc R
C6 C 0.2922(4) 0.14579(19) 0.2830(2) 0.0284(7) Uani 1 1 d .
H6 H 0.2925 0.1414 0.2249 0.034 Uiso 1 1 calc R
C7 C 0.1840(3) 0.1930(2) 0.3044(2) 0.0298(8) Uani 1 1 d .
H7 H 0.1094 0.2203 0.2611 0.036 Uiso 1 1 calc R
C8 C 0.1852(3) 0.20030(19) 0.38961(19) 0.0241(7) Uani 1 1 d .
H8 H 0.1126 0.2338 0.4047 0.029 Uiso 1 1 calc R
C9 C 0.1171(3) 0.13254(18) 0.57368(19) 0.0214(7) Uani 1 1 d .
C10 C -0.0098(3) 0.1806(2) 0.5440(2) 0.0301(8) Uani 1 1 d .
H10 H -0.0047 0.2354 0.5204 0.036 Uiso 1 1 calc R
C11 C -0.1448(4) 0.1486(2) 0.5487(2) 0.0423(10) Uani 1 1 d .
H11 H -0.2317 0.1813 0.5274 0.051 Uiso 1 1 calc R
C12 C -0.1523(4) 0.0702(3) 0.5839(3) 0.0463(10) Uani 1 1 d .
H12 H -0.2444 0.0488 0.5873 0.056 Uiso 1 1 calc R
C13 C -0.0268(5) 0.0222(2) 0.6144(2) 0.0445(10) Uani 1 1 d .
H13 H -0.0328 -0.0321 0.6387 0.053 Uiso 1 1 calc R
C14 C 0.1085(4) 0.05296(19) 0.6099(2) 0.0304(8) Uani 1 1 d .
H14 H 0.1949 0.0198 0.6314 0.036 Uiso 1 1 calc R
C15 C 0.5137(3) 0.31253(18) 0.55256(19) 0.0209(7) Uani 1 1 d .
H15 H 0.5268 0.2568 0.5332 0.025 Uiso 1 1 calc R
C16 C 0.6183(3) 0.37431(18) 0.55688(19) 0.0199(6) Uani 1 1 d .
H16 H 0.7033 0.3618 0.5389 0.024 Uiso 1 1 calc R
C17 C 0.6001(3) 0.45479(18) 0.58741(18) 0.0185(6) Uani 1 1 d .
H17 H 0.6721 0.4980 0.5921 0.022 Uiso 1 1 calc R
C18 C 0.5361(3) 0.61032(18) 0.68601(18) 0.0194(6) Uani 1 1 d .
C19 C 0.4487(3) 0.67334(18) 0.70325(19) 0.0210(6) Uani 1 1 d .
H19 H 0.4813 0.7256 0.7316 0.025 Uiso 1 1 calc R
C20 C 0.3038(3) 0.64700(17) 0.67176(18) 0.0180(6) Uani 1 1 d .
C21 C 0.1702(3) 0.69431(19) 0.6758(2) 0.0261(7) Uani 1 1 d .
H21A H 0.1079 0.7049 0.6177 0.039 Uiso 1 1 calc GR
H21B H 0.1990 0.7487 0.7051 0.039 Uiso 1 1 calc GR
H21C H 0.1154 0.6605 0.7073 0.039 Uiso 1 1 calc GR
C22 C 0.6999(3) 0.6035(2) 0.7125(2) 0.0268(7) Uani 1 1 d .
H22A H 0.7286 0.5455 0.7327 0.040 Uiso 1 1 calc GR
H22B H 0.7410 0.6441 0.7586 0.040 Uiso 1 1 calc GR
H22C H 0.7375 0.6162 0.6635 0.040 Uiso 1 1 calc GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Co Co 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 '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_3
Cl2 Co1 Cl2 84.59(3) 3_566
Cl1 Co1 Cl2 97.70(3) 3_566
Cl1 Co1 Cl2 114.84(3) .
N1 Co1 Cl2 119.57(7) .
N1 Co1 Cl2 100.14(7) 3_566
N1 Co1 Cl1 123.81(7) .
N1 Co1 N3 76.29(8) .
N3 Co1 Cl2 88.02(6) .
N3 Co1 Cl2 168.82(6) 3_566
N3 Co1 Cl1 93.01(6) .
Co1 Cl2 Co1 95.41(3) 3_566
N4 P1 S3 116.38(9) .
N4 P1 C3 103.91(12) .
N4 P1 C9 100.74(12) .
C3 P1 S3 111.98(10) .
C9 P1 S3 114.45(11) .
C9 P1 C3 108.25(13) .
N2 N1 Co1 115.47(16) .
C20 N1 Co1 138.43(19) .
C20 N1 N2 105.3(2) .
N1 N2 C1 118.5(2) .
C18 N2 N1 111.0(2) .
C18 N2 C1 130.5(2) .
C1 N3 Co1 111.20(17) .
C1 N3 C2 117.2(2) .
C2 N3 Co1 127.47(17) .
P1 N4 H4 117.6 .
C2 N4 P1 124.80(19) .
C2 N4 H4 117.6 .
N3 C1 N2 113.5(2) .
N3 C1 C17 124.6(3) .
C17 C1 N2 121.8(2) .
N3 C2 N4 115.1(2) .
N3 C2 C15 122.1(2) .
N4 C2 C15 122.8(2) .
C4 C3 P1 120.8(2) .
C4 C3 C8 119.2(3) .
C8 C3 P1 120.0(2) .
C3 C4 H4A 120.0 .
C5 C4 C3 120.1(3) .
C5 C4 H4A 120.0 .
C4 C5 H5 119.9 .
C6 C5 C4 120.3(3) .
C6 C5 H5 119.9 .
C5 C6 H6 119.7 .
C5 C6 C7 120.5(3) .
C7 C6 H6 119.7 .
C6 C7 H7 120.2 .
C6 C7 C8 119.6(3) .
C8 C7 H7 120.2 .
C3 C8 H8 119.9 .
C7 C8 C3 120.3(3) .
C7 C8 H8 119.9 .
C10 C9 P1 122.0(2) .
C10 C9 C14 119.2(3) .
C14 C9 P1 118.7(2) .
C9 C10 H10 119.9 .
C9 C10 C11 120.2(3) .
C11 C10 H10 119.9 .
C10 C11 H11 119.9 .
C12 C11 C10 120.1(4) .
C12 C11 H11 119.9 .
C11 C12 H12 119.9 .
C11 C12 C13 120.2(3) .
C13 C12 H12 119.9 .
C12 C13 H13 119.8 .
C12 C13 C14 120.4(3) .
C14 C13 H13 119.8 .
C9 C14 H14 120.1 .
C13 C14 C9 119.8(3) .
C13 C14 H14 120.1 .
C2 C15 H15 120.6 .
C16 C15 C2 118.8(3) .
C16 C15 H15 120.6 .
C15 C16 H16 119.9 .
C15 C16 C17 120.2(3) .
C17 C16 H16 119.9 .
C1 C17 C16 116.9(3) .
C1 C17 H17 121.6 .
C16 C17 H17 121.6 .
N2 C18 C19 105.9(2) .
N2 C18 C22 124.7(3) .
C19 C18 C22 129.2(3) .
C18 C19 H19 126.3 .
C18 C19 C20 107.5(3) .
C20 C19 H19 126.3 .
N1 C20 C19 110.3(2) .
N1 C20 C21 122.7(2) .
C19 C20 C21 127.0(3) .
C20 C21 H21A 109.5 .
C20 C21 H21B 109.5 .
C20 C21 H21C 109.5 .
H21A C21 H21B 109.5 .
H21A C21 H21C 109.5 .
H21B C21 H21C 109.5 .
C18 C22 H22A 109.5 .
C18 C22 H22B 109.5 .
C18 C22 H22C 109.5 .
H22A C22 H22B 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Cl2 2.3429(8) .
Co1 Cl2 2.4648(8) 3_566
Co1 Cl1 2.2656(9) .
Co1 N1 2.041(2) .
Co1 N3 2.243(2) .
Cl2 Co1 2.4647(8) 3_566
S3 P1 1.9364(11) .
P1 N4 1.686(2) .
P1 C3 1.811(3) .
P1 C9 1.807(3) .
N1 N2 1.379(3) .
N1 C20 1.340(3) .
N2 C1 1.414(3) .
N2 C18 1.367(3) .
N3 C1 1.340(3) .
N3 C2 1.347(3) .
N4 H4 0.8811 .
N4 C2 1.387(3) .
C1 C17 1.384(4) .
C2 C15 1.397(4) .
C3 C4 1.392(4) .
C3 C8 1.394(4) .
C4 H4A 0.9500 .
C4 C5 1.388(4) .
C5 H5 0.9500 .
C5 C6 1.370(4) .
C6 H6 0.9500 .
C6 C7 1.386(4) .
C7 H7 0.9500 .
C7 C8 1.390(4) .
C8 H8 0.9500 .
C9 C10 1.387(4) .
C9 C14 1.395(4) .
C10 H10 0.9500 .
C10 C11 1.395(4) .
C11 H11 0.9500 .
C11 C12 1.369(5) .
C12 H12 0.9500 .
C12 C13 1.377(5) .
C13 H13 0.9500 .
C13 C14 1.390(5) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C15 C16 1.374(4) .
C16 H16 0.9500 .
C16 C17 1.387(4) .
C17 H17 0.9500 .
C18 C19 1.369(4) .
C18 C22 1.493(4) .
C19 H19 0.9500 .
C19 C20 1.387(4) .
C20 C21 1.484(4) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
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
Co1 N1 N2 C1 8.2(3)
Co1 N1 N2 C18 -169.97(18)
Co1 N1 C20 C19 167.6(2)
Co1 N1 C20 C21 -12.4(5)
Co1 N3 C1 N2 24.4(3)
Co1 N3 C1 C17 -154.4(2)
Co1 N3 C2 N4 -30.4(3)
Co1 N3 C2 C15 151.0(2)
S3 P1 N4 C2 55.2(3)
S3 P1 C3 C4 3.9(3)
S3 P1 C3 C8 -175.5(2)
S3 P1 C9 C10 160.9(2)
S3 P1 C9 C14 -21.0(3)
P1 N4 C2 N3 -169.43(19)
P1 N4 C2 C15 9.2(4)
P1 C3 C4 C5 -178.3(2)
P1 C3 C8 C7 180.0(2)
P1 C9 C10 C11 176.6(3)
P1 C9 C14 C13 -177.0(2)
N1 N2 C1 N3 -22.8(3)
N1 N2 C1 C17 156.0(2)
N1 N2 C18 C19 -1.7(3)
N1 N2 C18 C22 174.1(3)
N2 N1 C20 C19 -0.8(3)
N2 N1 C20 C21 179.2(3)
N2 C1 C17 C16 179.5(3)
N2 C18 C19 C20 1.1(3)
N3 C1 C17 C16 -1.9(4)
N3 C2 C15 C16 1.1(4)
N4 P1 C3 C4 130.3(2)
N4 P1 C3 C8 -49.1(3)
N4 P1 C9 C10 35.3(3)
N4 P1 C9 C14 -146.7(2)
N4 C2 C15 C16 -177.5(3)
C1 N2 C18 C19 -179.5(3)
C1 N2 C18 C22 -3.7(5)
C1 N3 C2 N4 174.5(2)
C1 N3 C2 C15 -4.1(4)
C2 N3 C1 N2 -176.6(2)
C2 N3 C1 C17 4.6(4)
C2 C15 C16 C17 1.8(4)
C3 P1 N4 C2 -68.4(2)
C3 P1 C9 C10 -73.4(3)
C3 P1 C9 C14 104.7(3)
C3 C4 C5 C6 -1.8(4)
C4 C3 C8 C7 0.6(4)
C4 C5 C6 C7 0.8(5)
C5 C6 C7 C8 0.9(5)
C6 C7 C8 C3 -1.6(4)
C8 C3 C4 C5 1.1(4)
C9 P1 N4 C2 179.5(2)
C9 P1 C3 C4 -123.2(2)
C9 P1 C3 C8 57.4(3)
C9 C10 C11 C12 1.1(5)
C10 C9 C14 C13 1.1(5)
C10 C11 C12 C13 -0.4(6)
C11 C12 C13 C14 0.1(6)
C12 C13 C14 C9 -0.4(5)
C14 C9 C10 C11 -1.5(5)
C15 C16 C17 C1 -1.4(4)
C18 N2 C1 N3 154.9(3)
C18 N2 C1 C17 -26.3(4)
C18 C19 C20 N1 -0.2(3)
C18 C19 C20 C21 179.9(3)
C20 N1 N2 C1 179.7(2)
C20 N1 N2 C18 1.5(3)
C22 C18 C19 C20 -174.4(3)
