#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/30/4323011.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_4323011
loop_
_publ_author_name
'Lluis Escriche'
'José Antonio Muñoz'
'Joan Rosell'
'Raikko Kivekäs'
'Reijo Sillanpää'
'Jaume Casabó'
_publ_contact_author
;    Prof. Lluis Escriche
     Departament de Quìmica
     Universitat Autónoma de Barcelona
     08193 Bellaterra
     Barcelona
     Spain
;
_publ_contact_author_email       iqicasabo@cc.uab.es
_publ_contact_author_fax         '34 3 5813101'
_publ_contact_author_phone       '34 3 5811606'
_publ_section_title
;
 Synthesis and Reactivity of Nickel(II) Complexes of the Pyridine-Based
 Phosphorus-Containing Macrocycle 6-Phenyl-15-aza-6-phospha-3,9-
 dithiabicyclo[9,3,1]pentadeca-1(15),11,13-triene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4807
_journal_page_last               4813
_journal_paper_doi               10.1021/ic9714753
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C34 H40 N2 Ni O2 P2 S4, 2(Cl O4)'
_chemical_formula_structural     'C34 H40 N2 Ni O2 P2 S4, (Cl O4)2'
_chemical_formula_sum            'C34 H40 Cl2 N2 Ni O10 P2 S4'
_chemical_formula_weight         956.47
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             97-00-12
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                109.79(1)
_cell_angle_beta                 95.67(2)
_cell_angle_gamma                109.19(1)
_cell_formula_units_Z            1
_cell_length_a                   10.564(1)
_cell_length_b                   11.975(2)
_cell_length_c                   9.124(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      17.8
_cell_measurement_theta_min      14.0
_cell_volume                     996.6(3)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1993)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1993)
;
_computing_data_reduction
;
Texsan Process (Molecular Structure Corporation ,1993)
;
_computing_molecular_graphics    xtal_ORTEP
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  'xtal_CRYLSQ (Hall, Flack & Stewart, 1992)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3717
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.97
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.466
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.576
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2658
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .059
_refine_ls_shift/esd_max         .012
_refine_ls_shift/esd_mean        .003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         .067
_reflns_d_resolution_high        .841
_reflns_d_resolution_low         10.391
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_observed          2658
_reflns_number_total             3508
_reflns_observed_criterion       refl_observed_if_F____>_4__sigma(F___)
_cod_data_source_file            ic9714753_3.cif
_cod_data_source_block           compound_2_for_IC9714753
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_geom_bond_publ_flag' value
'Y' changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (20 times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               4323011
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
Ni1 1.00000 1.00000 .50000 .0291(4) Uani ? ?
Cl1 .7252(2) 1.3955(2) .2476(2) .0566(8) Uani ? ?
S1 .9869(2) 1.1000(2) .3079(2) .0380(7) Uani ? ?
S2 .5430(2) .8654(2) .5184(2) .0508(8) Uani ? ?
P1 .7207(2) .8024(2) .2212(2) .0363(7) Uani ? ?
O1 .8369(4) .8364(4) .3602(5) .036(2) Uani ? ?
O2 .8564(8) 1.4206(9) .330(1) .115(5) Uani ? ?
O3 .6492(8) 1.437(1) .3545(9) .128(5) Uani ? ?
O4 .740(1) 1.464(1) .149(1) .178(8) Uani ? ?
O5 .655(1) 1.2680(9) .141(1) .145(5) Uani ? ?
N1 .8641(5) 1.0983(5) .5881(6) .033(2) Uani ? ?
C1 .9860(7) 1.2408(6) .4626(9) .043(3) Uani ? ?
C2 .9019(7) 1.2138(6) .5802(8) .037(3) Uani ? ?
C3 .8670(8) 1.3108(7) .6781(9) .050(3) Uani ? ?
C4 .7926(8) 1.2886(8) .786(1) .060(4) Uani ? ?
C5 .7442(7) 1.1667(8) .7872(9) .050(3) Uani ? ?
C6 .7785(7) 1.0729(7) .6840(8) .042(3) Uani ? ?
C7 .7084(7) .9355(7) .6635(8) .045(3) Uani ? ?
C8 .5382(8) .7083(7) .396(1) .052(3) Uani ? ?
C9 .5605(7) .6913(7) .2309(9) .050(3) Uani ? ?
C10 .6966(7) .9417(7) .2108(8) .044(3) Uani ? ?
C11 .8173(7) 1.0320(7) .1733(8) .044(3) Uani ? ?
C12 .7574(7) .7269(6) .0339(8) .040(3) Uani ? ?
C13 .8781(8) .7079(8) .0299(9) .051(3) Uani ? ?
C14 .9063(9) .6488(8) -.116(1) .058(4) Uani ? ?
C15 .8112(8) .6063(7) -.2560(8) .048(3) Uani ? ?
C16 .6913(8) .6243(7) -.2555(9) .050(3) Uani ? ?
C17 .6630(8) .6855(7) -.1094(8) .048(3) Uani ? ?
H1A 1.07855 1.29408 .52078 .07000 Uiso ? ?
H1B .94964 1.28528 .41280 .07000 Uiso ? ?
H3 .89475 1.39196 .66982 .07000 Uiso ? ?
H4 .77409 1.35600 .85960 .07000 Uiso ? ?
H5 .68830 1.14795 .85799 .07000 Uiso ? ?
H7A .76410 .88905 .62523 .07000 Uiso ? ?
H7B .69366 .93235 .76332 .07000 Uiso ? ?
H8A .60808 .69332 .45132 .07000 Uiso ? ?
H8B .45047 .64591 .38524 .07000 Uiso ? ?
H9A .55758 .60665 .17971 .07000 Uiso ? ?
H9B .48699 .70053 .17386 .07000 Uiso ? ?
H10A .61620 .91310 .12930 .07000 Uiso ? ?
H10B .68358 .98885 .31119 .07000 Uiso ? ?
H11A .82502 .98513 .06960 .07000 Uiso ? ?
H11B .79419 1.10189 .17171 .07000 Uiso ? ?
H13 .94307 .73515 .12728 .07000 Uiso ? ?
H14 .99137 .63798 -.11794 .07000 Uiso ? ?
H15 .82959 .56360 -.35495 .07000 Uiso ? ?
H16 .62664 .59555 -.35359 .07000 Uiso ? ?
H17 .57908 .69859 -.10845 .07000 Uiso ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0 1 .284973 1.113 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
Cl Cl 0 2 .132019 .158997 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
S S 0 4 .109985 .124023 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
P P 0 2 .090027 .094971 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
O O 0 10 .007996 .005981 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
N N 0 2 .004028 .002991 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
C C 0 34 .002014 .002014 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
H H 0 40 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 O1 92.8(2) . . . y
S1 Ni1 N1 79.8(2) . . . y
S1 Ni1 S1 180.0000 . . 2_776 ?
S1 Ni1 O1 87.2(2) . . 2_776 ?
S1 Ni1 N1 100.2(2) . . 2_776 ?
O1 Ni1 N1 91.5(2) . . . y
O1 Ni1 S1 87.2(2) . . 2_776 ?
O1 Ni1 O1 180.0(2) . . 2_776 ?
O1 Ni1 N1 88.5(2) . . 2_776 ?
N1 Ni1 S1 100.2(2) . . 2_776 ?
N1 Ni1 O1 88.5(2) . . 2_776 ?
N1 Ni1 N1 180.0000 . . 2_776 ?
S1 Ni1 O1 92.8(2) 2_776 . 2_776 ?
S1 Ni1 N1 79.8(2) 2_776 . 2_776 ?
O1 Ni1 N1 91.5(2) 2_776 . 2_776 ?
Ni1 S1 C1 90.9(3) . . . y
Ni1 S1 C11 113.5(3) . . . y
C1 S1 C11 103.5(4) . . . y
C7 S2 C8 102.0(4) . . . y
O1 P1 C9 111.0(4) . . . y
O1 P1 C10 112.8(3) . . . y
O1 P1 C12 110.9(3) . . . y
C9 P1 C10 109.5(4) . . . y
C9 P1 C12 107.4(3) . . . y
C10 P1 C12 105.1(4) . . . y
Ni1 O1 P1 133.8(3) . . . y
Ni1 N1 C2 112.2(5) . . . ?
Ni1 N1 C6 126.9(6) . . . ?
C2 N1 C6 118.1(6) . . . ?
S1 C1 C2 114.7(5) . . . y
S1 C1 H1A 108.1(7) . . . ?
S1 C1 H1B 108.1(5) . . . ?
C2 C1 H1A 108.1(6) . . . ?
C2 C1 H1B 108.1(8) . . . ?
H1A C1 H1B 109.5(7) . . . ?
N1 C2 C1 119.4(6) . . . ?
N1 C2 C3 122.0(7) . . . ?
C1 C2 C3 118.6(7) . . . ?
C2 C3 C4 119.4(8) . . . ?
C2 C3 H3 120.3(9) . . . ?
C4 C3 H3 120.3(9) . . . ?
C3 C4 C5 119.2(8) . . . ?
C3 C4 H4 120.4(9) . . . ?
C5 C4 H4 120.4(9) . . . ?
C4 C5 C6 118.9(8) . . . ?
C4 C5 H5 120.6(9) . . . ?
C6 C5 H5 120.6(9) . . . ?
N1 C6 C5 122.0(7) . . . ?
N1 C6 C7 118.2(6) . . . ?
C5 C6 C7 119.5(7) . . . ?
S2 C7 C6 108.2(6) . . . y
S2 C7 H7A 109.8(5) . . . ?
S2 C7 H7B 109.8(5) . . . ?
C6 C7 H7A 109.8(7) . . . ?
C6 C7 H7B 109.8(6) . . . ?
H7A C7 H7B 109.5(9) . . . ?
S2 C8 C9 115.4(7) . . . y
S2 C8 H8A 108.0(5) . . . ?
S2 C8 H8B 108.0(7) . . . ?
C9 C8 H8A 108.0(8) . . . ?
C9 C8 H8B 108.0(6) . . . ?
H8A C8 H8B 109(1) . . . ?
P1 C9 C8 116.1(4) . . . y
P1 C9 H9A 107.8(6) . . . ?
P1 C9 H9B 107.8(7) . . . ?
C8 C9 H9A 107.8(8) . . . ?
C8 C9 H9B 107.8(8) . . . ?
H9A C9 H9B 109.5(6) . . . ?
P1 C10 C11 114.3(6) . . . y
P1 C10 H10A 108.3(5) . . . ?
P1 C10 H10B 108.3(7) . . . ?
C11 C10 H10A 108.3(8) . . . ?
C11 C10 H10B 108.3(6) . . . ?
H10A C10 H10B 109.5(8) . . . ?
S1 C11 C10 118.2(6) . . . y
S1 C11 H11A 107.2(6) . . . ?
S1 C11 H11B 107.2(4) . . . ?
C10 C11 H11A 107.2(5) . . . ?
C10 C11 H11B 107.2(7) . . . ?
H11A C11 H11B 109.5(9) . . . ?
P1 C12 C13 120.5(5) . . . ?
P1 C12 C17 120.4(6) . . . ?
C13 C12 C17 119.0(7) . . . ?
C12 C13 C14 120.5(7) . . . ?
C12 C13 H13 119.8(8) . . . ?
C14 C13 H13 119.8(9) . . . ?
C13 C14 C15 119.8(9) . . . ?
C13 C14 H14 120.1(8) . . . ?
C15 C14 H14 120.1(8) . . . ?
C14 C15 C16 120.9(8) . . . ?
C14 C15 H15 119.5(9) . . . ?
C16 C15 H15 119.5(7) . . . ?
C15 C16 C17 119.6(7) . . . ?
C15 C16 H16 120.2(8) . . . ?
C17 C16 H16 120.2(9) . . . ?
C12 C17 C16 120.1(8) . . . ?
C12 C17 H17 119.9(7) . . . ?
C16 C17 H17 119.9(7) . . . ?
O2 Cl1 O3 110.6(5) . . . ?
O2 Cl1 O4 108.2(7) . . . ?
O2 Cl1 O5 113.6(7) . . . ?
O3 Cl1 O4 108.0(8) . . . ?
O3 Cl1 O5 112.2(6) . . . ?
O4 Cl1 O5 103.9(6) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.451(2) . . y
Ni1 O1 2.022(3) . . y
Ni1 N1 2.189(6) . . y
Ni1 S1 2.451(2) . 2_776 ?
Ni1 O1 2.022(3) . 2_776 ?
Ni1 N1 2.189(6) . 2_776 ?
S1 C1 1.799(7) . . y
S1 C11 1.819(7) . . y
S2 C7 1.827(7) . . y
S2 C8 1.814(8) . . y
P1 O1 1.515(5) . . y
P1 C9 1.809(7) . . y
P1 C10 1.799(9) . . y
P1 C12 1.789(7) . . y
N1 C2 1.34(1) . . y
N1 C6 1.35(1) . . y
C1 C2 1.51(1) . . y
C1 H1A .950(6) . . ?
C1 H1B .950(9) . . ?
C2 C3 1.39(1) . . ?
C3 C4 1.36(1) . . ?
C3 H3 .950(9) . . ?
C4 C5 1.38(1) . . ?
C4 H4 .950(9) . . ?
C5 C6 1.38(1) . . ?
C5 H5 .950(8) . . ?
C6 C7 1.50(1) . . y
C7 H7A .950(9) . . ?
C7 H7B .950(8) . . ?
C8 C9 1.51(1) . . y
C8 H8A .95(1) . . ?
C8 H8B .950(7) . . ?
C9 H9A .950(8) . . ?
C9 H9B .950(9) . . ?
C10 C11 1.53(1) . . y
C10 H10A .950(7) . . ?
C10 H10B .950(7) . . ?
C11 H11A .950(7) . . ?
C11 H11B .950(9) . . ?
C12 C13 1.37(1) . . ?
C12 C17 1.39(1) . . ?
C13 C14 1.39(1) . . ?
C13 H13 .950(8) . . ?
C14 C15 1.37(1) . . ?
C14 H14 .95(1) . . ?
C15 C16 1.35(1) . . ?
C15 H15 .950(8) . . ?
C16 C17 1.40(1) . . ?
C16 H16 .950(8) . . ?
C17 H17 .950(9) . . ?
Cl1 O2 1.394(9) . . ?
Cl1 O3 1.390(9) . . ?
Cl1 O4 1.40(2) . . ?
Cl1 O5 1.392(8) . . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
loop_
_reflns_scale_group_code
_reflns_scale_meas_F
? .408509
