#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:23:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180137 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/34/7103435.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_7103435
loop_
_publ_author_name
'Guironnet, Damien'
'Rünzi, Thomas'
'Göttker-Schnetmann, Inigo'
'Mecking, Stefan'
_publ_section_title
;
 Control of molecular weight in Ni(II)-catalyzed polymerization via the
 reaction medium.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4965
_journal_page_last               4967
_journal_paper_doi               10.1039/b811888d
_journal_year                    2008
_chemical_formula_moiety         'C26 H26 N Ni O5 P S'
_chemical_formula_sum            'C26 H26 N Ni O5 P S'
_chemical_formula_weight         554.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 98.617(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4740(7)
_cell_length_b                   13.8165(6)
_cell_length_c                   16.0318(10)
_cell_measurement_reflns_used    41670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      1.84
_cell_volume                     2512.8(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41727
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.7235
_exptl_absorpt_correction_T_min  0.5945
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-SHAPE'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0363
_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)+(0.0344P)²+1.8600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                5141
_reflns_number_total             6018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811888d.txt
_cod_data_source_block           dg01a_drent1_nimepyr
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7103435
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.73707(2) 0.035276(18) 0.168493(15) 0.01534(7) Uani 1 1 d . . .
P3 P 0.68713(4) 0.11921(3) 0.27108(3) 0.01299(10) Uani 1 1 d . . .
S3 S 0.94990(4) 0.17227(3) 0.22327(3) 0.01424(10) Uani 1 1 d . . .
O2 O 0.98711(12) 0.11696(10) 0.29912(9) 0.0194(3) Uani 1 1 d . . .
O3 O 0.87712(12) 0.11378(10) 0.15719(9) 0.0180(3) Uani 1 1 d . . .
O4 O 1.04364(12) 0.22055(11) 0.18892(9) 0.0208(3) Uani 1 1 d . . .
O5 O 0.71158(14) 0.19445(11) 0.44965(9) 0.0239(3) Uani 1 1 d . . .
N6 N 0.79629(15) -0.05142(12) 0.08969(11) 0.0191(3) Uani 1 1 d . . .
O7 O 0.50198(13) 0.20538(12) 0.14759(10) 0.0267(3) Uani 1 1 d . . .
C7 C 0.74341(16) 0.24352(14) 0.27306(12) 0.0142(3) Uani 1 1 d . . .
C8 C 0.85404(16) 0.26491(14) 0.24938(11) 0.0141(3) Uani 1 1 d . . .
C9 C 0.67483(17) 0.32139(14) 0.29322(13) 0.0184(4) Uani 1 1 d . . .
H9 H 0.6002 0.3091 0.3100 0.022 Uiso 1 1 calc R . .
C10 C 0.37029(18) 0.11140(17) 0.36099(15) 0.0264(5) Uani 1 1 d . . .
H10 H 0.3416 0.0891 0.4102 0.032 Uiso 1 1 calc R . .
C11 C 0.75334(16) 0.06131(14) 0.36841(12) 0.0169(4) Uani 1 1 d . . .
C12 C 0.48849(17) 0.10001(15) 0.35277(14) 0.0211(4) Uani 1 1 d . . .
H12 H 0.5402 0.0688 0.3964 0.025 Uiso 1 1 calc R . .
C13 C 0.76290(17) 0.10570(15) 0.44801(13) 0.0201(4) Uani 1 1 d . . .
C14 C 0.9020(2) -0.19687(16) 0.07145(14) 0.0267(5) Uani 1 1 d . . .
H14 H 0.9298 -0.2580 0.0930 0.032 Uiso 1 1 calc R . .
C15 C 0.89299(17) 0.35996(14) 0.24606(12) 0.0170(4) Uani 1 1 d . . .
H15 H 0.9680 0.3730 0.2304 0.020 Uiso 1 1 calc R . .
C16 C 0.53247(16) 0.13358(14) 0.28164(13) 0.0172(4) Uani 1 1 d . . .
C17 C 0.59690(19) -0.04215(17) 0.16773(16) 0.0289(5) Uani 1 1 d . . .
H17A H 0.5311 -0.0118 0.1310 0.035 Uiso 1 1 calc R . .
H17B H 0.5779 -0.0468 0.2252 0.035 Uiso 1 1 calc R . .
H17C H 0.6106 -0.1071 0.1467 0.035 Uiso 1 1 calc R . .
C18 C 0.8558(2) -0.07909(17) 0.43450(15) 0.0286(5) Uani 1 1 d . . .
H18 H 0.8865 -0.1424 0.4301 0.034 Uiso 1 1 calc R . .
C19 C 0.82257(18) 0.43572(15) 0.26561(13) 0.0204(4) Uani 1 1 d . . .
H19 H 0.8489 0.5007 0.2628 0.024 Uiso 1 1 calc R . .
C20 C 0.8356(2) -0.13906(15) 0.11657(13) 0.0229(4) Uani 1 1 d . . .
H20 H 0.8169 -0.1624 0.1688 0.027 Uiso 1 1 calc R . .
C21 C 0.29539(18) 0.15540(16) 0.29698(16) 0.0272(5) Uani 1 1 d . . .
H21 H 0.2148 0.1638 0.3027 0.033 Uiso 1 1 calc R . .
C22 C 0.8204(2) -0.02152(16) 0.01430(14) 0.0264(5) Uani 1 1 d . . .
H22 H 0.7922 0.0400 -0.0061 0.032 Uiso 1 1 calc R . .
C23 C 0.80018(18) -0.03149(15) 0.36335(14) 0.0216(4) Uani 1 1 d . . .
H23 H 0.7938 -0.0626 0.3100 0.026 Uiso 1 1 calc R . .
C24 C 0.7260(2) 0.2448(2) 0.52791(16) 0.0360(6) Uani 1 1 d . . .
H24A H 0.8101 0.2556 0.5473 0.043 Uiso 1 1 calc R . .
H24B H 0.6925 0.2063 0.5698 0.043 Uiso 1 1 calc R . .
H24C H 0.6854 0.3073 0.5205 0.043 Uiso 1 1 calc R . .
C25 C 0.82010(19) 0.05862(18) 0.51948(14) 0.0275(5) Uani 1 1 d . . .
H25 H 0.8275 0.0894 0.5730 0.033 Uiso 1 1 calc R . .
C26 C 0.45387(18) 0.17643(15) 0.21640(14) 0.0214(4) Uani 1 1 d . . .
C27 C 0.9276(2) -0.16503(17) -0.00487(14) 0.0266(5) Uani 1 1 d . . .
H27 H 0.9741 -0.2032 -0.0366 0.032 Uiso 1 1 calc R . .
C28 C 0.8662(2) -0.03310(19) 0.51223(15) 0.0311(5) Uani 1 1 d . . .
H28 H 0.9053 -0.0649 0.5610 0.037 Uiso 1 1 calc R . .
C29 C 0.8841(2) -0.07629(17) -0.03455(15) 0.0306(5) Uani 1 1 d . . .
H29 H 0.8980 -0.0534 -0.0880 0.037 Uiso 1 1 calc R . .
C30 C 0.33525(18) 0.18770(16) 0.22444(16) 0.0258(5) Uani 1 1 d . . .
H30 H 0.2823 0.2172 0.1806 0.031 Uiso 1 1 calc R . .
C31 C 0.4244(2) 0.2480(3) 0.07933(19) 0.0525(8) Uani 1 1 d . . .
H31A H 0.3882 0.3061 0.0993 0.063 Uiso 1 1 calc R . .
H31B H 0.3627 0.2014 0.0578 0.063 Uiso 1 1 calc R . .
H31C H 0.4692 0.2656 0.0341 0.063 Uiso 1 1 calc R . .
C32 C 0.71357(18) 0.41622(15) 0.28919(14) 0.0211(4) Uani 1 1 d . . .
H32 H 0.6652 0.4680 0.3027 0.025 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 '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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
C17 Ni1 N6 91.52(9) . . ?
C17 Ni1 O3 174.42(9) . . ?
N6 Ni1 O3 84.82(6) . . ?
C17 Ni1 P3 89.23(7) . . ?
N6 Ni1 P3 171.28(5) . . ?
O3 Ni1 P3 95.03(4) . . ?
C11 P3 C16 104.86(9) . . ?
C11 P3 C7 107.27(9) . . ?
C16 P3 C7 104.02(9) . . ?
C11 P3 Ni1 107.06(7) . . ?
C16 P3 Ni1 120.24(7) . . ?
C7 P3 Ni1 112.54(6) . . ?
O4 S3 O2 114.98(9) . . ?
O4 S3 O3 110.54(8) . . ?
O2 S3 O3 112.08(9) . . ?
O4 S3 C8 106.25(9) . . ?
O2 S3 C8 107.31(8) . . ?
O3 S3 C8 104.95(8) . . ?
S3 O3 Ni1 127.82(8) . . ?
C13 O5 C24 117.63(18) . . ?
C20 N6 C22 117.52(18) . . ?
C20 N6 Ni1 118.88(14) . . ?
C22 N6 Ni1 122.40(14) . . ?
C26 O7 C31 117.29(19) . . ?
C9 C7 C8 117.47(17) . . ?
C9 C7 P3 121.03(14) . . ?
C8 C7 P3 121.38(14) . . ?
C15 C8 C7 121.05(17) . . ?
C15 C8 S3 117.20(14) . . ?
C7 C8 S3 121.76(14) . . ?
C32 C9 C7 121.33(18) . . ?
C21 C10 C12 119.2(2) . . ?
C23 C11 C13 118.35(18) . . ?
C23 C11 P3 118.00(15) . . ?
C13 C11 P3 123.63(16) . . ?
C10 C12 C16 121.2(2) . . ?
O5 C13 C25 123.8(2) . . ?
O5 C13 C11 115.80(18) . . ?
C25 C13 C11 120.4(2) . . ?
C27 C14 C20 119.3(2) . . ?
C19 C15 C8 120.18(18) . . ?
C12 C16 C26 118.59(18) . . ?
C12 C16 P3 121.19(15) . . ?
C26 C16 P3 120.20(15) . . ?
C23 C18 C28 119.2(2) . . ?
C32 C19 C15 119.68(19) . . ?
N6 C20 C14 122.6(2) . . ?
C10 C21 C30 121.33(19) . . ?
N6 C22 C29 122.8(2) . . ?
C18 C23 C11 121.4(2) . . ?
C28 C25 C13 119.8(2) . . ?
O7 C26 C30 124.1(2) . . ?
O7 C26 C16 115.64(17) . . ?
C30 C26 C16 120.3(2) . . ?
C14 C27 C29 118.5(2) . . ?
C25 C28 C18 120.8(2) . . ?
C22 C29 C27 119.2(2) . . ?
C21 C30 C26 119.4(2) . . ?
C19 C32 C9 120.29(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C17 1.930(2) . ?
Ni1 N6 1.9364(17) . ?
Ni1 O3 1.9695(14) . ?
Ni1 P3 2.1587(5) . ?
P3 C11 1.816(2) . ?
P3 C16 1.8186(19) . ?
P3 C7 1.8336(19) . ?
S3 O4 1.4430(14) . ?
S3 O2 1.4456(14) . ?
S3 O3 1.4858(14) . ?
S3 C8 1.7780(19) . ?
O5 C13 1.362(3) . ?
O5 C24 1.423(3) . ?
N6 C20 1.340(3) . ?
N6 C22 1.345(3) . ?
O7 C26 1.365(3) . ?
O7 C31 1.430(3) . ?
C7 C9 1.399(3) . ?
C7 C8 1.410(2) . ?
C8 C15 1.391(3) . ?
C9 C32 1.388(3) . ?
C10 C21 1.377(3) . ?
C10 C12 1.391(3) . ?
C11 C23 1.397(3) . ?
C11 C13 1.405(3) . ?
C12 C16 1.394(3) . ?
C13 C25 1.393(3) . ?
C14 C27 1.372(3) . ?
C14 C20 1.382(3) . ?
C15 C19 1.386(3) . ?
C16 C26 1.405(3) . ?
C18 C23 1.387(3) . ?
C18 C28 1.388(4) . ?
C19 C32 1.386(3) . ?
C21 C30 1.386(3) . ?
C22 C29 1.376(3) . ?
C25 C28 1.385(4) . ?
C26 C30 1.395(3) . ?
C27 C29 1.381(3) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C17 Ni1 P3 C11 90.37(10) . . . . ?
N6 Ni1 P3 C11 -4.6(4) . . . . ?
O3 Ni1 P3 C11 -93.24(8) . . . . ?
C17 Ni1 P3 C16 -28.94(11) . . . . ?
N6 Ni1 P3 C16 -124.0(4) . . . . ?
O3 Ni1 P3 C16 147.44(9) . . . . ?
C17 Ni1 P3 C7 -152.01(10) . . . . ?
N6 Ni1 P3 C7 113.0(4) . . . . ?
O3 Ni1 P3 C7 24.38(8) . . . . ?
O4 S3 O3 Ni1 -178.92(10) . . . . ?
O2 S3 O3 Ni1 51.39(13) . . . . ?
C8 S3 O3 Ni1 -64.75(12) . . . . ?
C17 Ni1 O3 S3 166.1(8) . . . . ?
N6 Ni1 O3 S3 -144.72(12) . . . . ?
P3 Ni1 O3 S3 26.52(11) . . . . ?
C17 Ni1 N6 C20 -71.91(18) . . . . ?
O3 Ni1 N6 C20 112.31(16) . . . . ?
P3 Ni1 N6 C20 22.9(5) . . . . ?
C17 Ni1 N6 C22 120.92(19) . . . . ?
O3 Ni1 N6 C22 -54.86(18) . . . . ?
P3 Ni1 N6 C22 -144.2(3) . . . . ?
C11 P3 C7 C9 -101.60(17) . . . . ?
C16 P3 C7 C9 9.16(18) . . . . ?
Ni1 P3 C7 C9 140.89(14) . . . . ?
C11 P3 C7 C8 82.35(17) . . . . ?
C16 P3 C7 C8 -166.89(15) . . . . ?
Ni1 P3 C7 C8 -35.16(17) . . . . ?
C9 C7 C8 C15 -0.2(3) . . . . ?
P3 C7 C8 C15 176.01(14) . . . . ?
C9 C7 C8 S3 179.40(14) . . . . ?
P3 C7 C8 S3 -4.4(2) . . . . ?
O4 S3 C8 C15 -9.93(17) . . . . ?
O2 S3 C8 C15 113.55(15) . . . . ?
O3 S3 C8 C15 -127.06(15) . . . . ?
O4 S3 C8 C7 170.48(15) . . . . ?
O2 S3 C8 C7 -66.05(17) . . . . ?
O3 S3 C8 C7 53.34(17) . . . . ?
C8 C7 C9 C32 0.7(3) . . . . ?
P3 C7 C9 C32 -175.50(16) . . . . ?
C16 P3 C11 C23 116.01(16) . . . . ?
C7 P3 C11 C23 -133.81(15) . . . . ?
Ni1 P3 C11 C23 -12.78(16) . . . . ?
C16 P3 C11 C13 -65.81(18) . . . . ?
C7 P3 C11 C13 44.37(18) . . . . ?
Ni1 P3 C11 C13 165.40(15) . . . . ?
C21 C10 C12 C16 1.0(3) . . . . ?
C24 O5 C13 C25 5.4(3) . . . . ?
C24 O5 C13 C11 -175.82(19) . . . . ?
C23 C11 C13 O5 -177.46(17) . . . . ?
P3 C11 C13 O5 4.4(2) . . . . ?
C23 C11 C13 C25 1.4(3) . . . . ?
P3 C11 C13 C25 -176.80(15) . . . . ?
C7 C8 C15 C19 -0.4(3) . . . . ?
S3 C8 C15 C19 179.95(15) . . . . ?
C10 C12 C16 C26 -2.3(3) . . . . ?
C10 C12 C16 P3 179.71(16) . . . . ?
C11 P3 C16 C12 -1.82(19) . . . . ?
C7 P3 C16 C12 -114.33(17) . . . . ?
Ni1 P3 C16 C12 118.59(15) . . . . ?
C11 P3 C16 C26 -179.81(16) . . . . ?
C7 P3 C16 C26 67.68(17) . . . . ?
Ni1 P3 C16 C26 -59.40(18) . . . . ?
C8 C15 C19 C32 0.6(3) . . . . ?
C22 N6 C20 C14 2.2(3) . . . . ?
Ni1 N6 C20 C14 -165.56(18) . . . . ?
C27 C14 C20 N6 -1.3(4) . . . . ?
C12 C10 C21 C30 0.6(3) . . . . ?
C20 N6 C22 C29 -0.9(3) . . . . ?
Ni1 N6 C22 C29 166.42(19) . . . . ?
C28 C18 C23 C11 -0.6(3) . . . . ?
C13 C11 C23 C18 -0.5(3) . . . . ?
P3 C11 C23 C18 177.73(16) . . . . ?
O5 C13 C25 C28 177.73(19) . . . . ?
C11 C13 C25 C28 -1.0(3) . . . . ?
C31 O7 C26 C30 -1.3(3) . . . . ?
C31 O7 C26 C16 179.1(2) . . . . ?
C12 C16 C26 O7 -178.30(18) . . . . ?
P3 C16 C26 O7 -0.3(3) . . . . ?
C12 C16 C26 C30 2.1(3) . . . . ?
P3 C16 C26 C30 -179.87(16) . . . . ?
C20 C14 C27 C29 -0.9(4) . . . . ?
C13 C25 C28 C18 -0.2(3) . . . . ?
C23 C18 C28 C25 1.0(3) . . . . ?
N6 C22 C29 C27 -1.3(4) . . . . ?
C14 C27 C29 C22 2.2(4) . . . . ?
C10 C21 C30 C26 -0.7(3) . . . . ?
O7 C26 C30 C21 179.8(2) . . . . ?
C16 C26 C30 C21 -0.6(3) . . . . ?
C15 C19 C32 C9 -0.1(3) . . . . ?
C7 C9 C32 C19 -0.6(3) . . . . ?
