#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:56:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179162 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/23/4312312.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_4312312
loop_
_publ_author_name
'Donald J. Darensbourg'
'Cesar G. Ortiz'
'Jason C. Yarbrough'
_publ_section_title
;
 Synthesis and Structures of Nickel and Palladium Salicylaldiminato
 1,3,5-Triaza-7-phosphaadamantane (PTA) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6915
_journal_page_last               6922
_journal_paper_doi               10.1021/ic0341284
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C41 H50 Cl2 N2 Ni O4'
_chemical_formula_weight         764.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.919(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9737(11)
_cell_length_b                   20.255(3)
_cell_length_c                   21.720(3)
_cell_measurement_temperature    110(2)
_cell_volume                     3947.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20750
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.121
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1069P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                3486
_reflns_number_total             8801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0341284si20030205_021052_4.cif
_cod_data_source_block           Structure5b'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3947.3(8)
_cod_database_code               4312312
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35841(5) 0.27423(2) 0.32013(2) 0.05219(19) Uani 1 1 d . . .
N1 N 0.3537(3) 0.36811(16) 0.31352(13) 0.0512(8) Uani 1 1 d . . .
N2 N 0.3686(3) 0.18028(15) 0.32479(12) 0.0441(7) Uani 1 1 d . . .
O1 O 0.4896(3) 0.27540(13) 0.38530(12) 0.0590(7) Uani 1 1 d . . .
O2 O 0.6590(3) 0.24571(17) 0.47937(13) 0.0758(9) Uani 1 1 d . . .
O3 O 0.2226(3) 0.27277(13) 0.25617(12) 0.0574(7) Uani 1 1 d . . .
O4 O 0.0406(3) 0.30061(15) 0.16505(13) 0.0714(8) Uani 1 1 d . . .
C2 C 0.4268(4) 0.4082(2) 0.34966(17) 0.0544(10) Uani 1 1 d . . .
H2 H 0.4175 0.4540 0.3408 0.065 Uiso 1 1 calc R . .
C3 C 0.5187(4) 0.3913(2) 0.40065(17) 0.0559(10) Uani 1 1 d . . .
C4 C 0.5857(5) 0.4420(2) 0.43680(18) 0.0664(12) Uani 1 1 d . . .
H4 H 0.5685 0.4868 0.4260 0.080 Uiso 1 1 calc R . .
C5 C 0.6740(5) 0.4278(2) 0.48663(19) 0.0700(13) Uani 1 1 d . . .
H5 H 0.7162 0.4624 0.5107 0.084 Uiso 1 1 calc R . .
C6 C 0.7022(5) 0.3619(3) 0.50209(19) 0.0685(12) Uani 1 1 d . . .
H6 H 0.7654 0.3521 0.5364 0.082 Uiso 1 1 calc R . .
C7 C 0.6399(4) 0.3107(2) 0.46849(18) 0.0594(11) Uani 1 1 d . . .
C8 C 0.5451(4) 0.3249(2) 0.41544(17) 0.0556(10) Uani 1 1 d . . .
C9 C 0.2715(4) 0.40076(19) 0.26363(18) 0.0532(10) Uani 1 1 d . . .
C10 C 0.3419(5) 0.4126(2) 0.20810(19) 0.0652(12) Uani 1 1 d . . .
C11 C 0.2624(7) 0.4454(2) 0.1622(2) 0.0842(16) Uani 1 1 d . . .
H11 H 0.3080 0.4538 0.1239 0.101 Uiso 1 1 calc R . .
C12 C 0.1191(7) 0.4657(3) 0.1714(3) 0.095(2) Uani 1 1 d . . .
H12 H 0.0672 0.4888 0.1396 0.114 Uiso 1 1 calc R . .
C13 C 0.0498(5) 0.4530(2) 0.2258(3) 0.0805(15) Uani 1 1 d . . .
H13 H -0.0500 0.4673 0.2310 0.097 Uiso 1 1 calc R . .
C14 C 0.1226(5) 0.4195(2) 0.2740(2) 0.0645(12) Uani 1 1 d . . .
C15 C 0.0446(5) 0.4051(2) 0.3328(2) 0.0793(14) Uani 1 1 d . . .
H15 H 0.1055 0.3716 0.3558 0.095 Uiso 1 1 calc R . .
C16 C -0.1093(6) 0.3756(3) 0.3217(3) 0.130(2) Uani 1 1 d . . .
H16A H -0.1743 0.4086 0.3021 0.194 Uiso 1 1 calc R . .
H16B H -0.1515 0.3621 0.3611 0.194 Uiso 1 1 calc R . .
H16C H -0.1013 0.3370 0.2947 0.194 Uiso 1 1 calc R . .
C17 C 0.0337(7) 0.4658(3) 0.3736(3) 0.1132(19) Uani 1 1 d . . .
H17A H 0.1341 0.4801 0.3861 0.170 Uiso 1 1 calc R . .
H17B H -0.0237 0.4550 0.4103 0.170 Uiso 1 1 calc R . .
H17C H -0.0162 0.5014 0.3507 0.170 Uiso 1 1 calc R . .
C18 C 0.4985(5) 0.3887(3) 0.1969(2) 0.0819(15) Uani 1 1 d . . .
H18 H 0.5389 0.3715 0.2370 0.098 Uiso 1 1 calc R . .
C19 C 0.4990(7) 0.3314(4) 0.1511(3) 0.156(3) Uani 1 1 d . . .
H19A H 0.4267 0.2979 0.1638 0.234 Uiso 1 1 calc R . .
H19B H 0.5987 0.3117 0.1502 0.234 Uiso 1 1 calc R . .
H19C H 0.4717 0.3477 0.1100 0.234 Uiso 1 1 calc R . .
C20 C 0.6024(7) 0.4430(4) 0.1762(3) 0.146(3) Uani 1 1 d . . .
H20A H 0.5683 0.4600 0.1361 0.219 Uiso 1 1 calc R . .
H20B H 0.7035 0.4253 0.1725 0.219 Uiso 1 1 calc R . .
H20C H 0.6027 0.4789 0.2065 0.219 Uiso 1 1 calc R . .
C21 C 0.7684(5) 0.2282(2) 0.5253(2) 0.0867(16) Uani 1 1 d . . .
H21A H 0.8666 0.2438 0.5126 0.130 Uiso 1 1 calc R . .
H21B H 0.7706 0.1801 0.5301 0.130 Uiso 1 1 calc R . .
H21C H 0.7427 0.2487 0.5646 0.130 Uiso 1 1 calc R . .
C22 C 0.3035(4) 0.1400(2) 0.28712(17) 0.0519(10) Uani 1 1 d . . .
H22 H 0.3211 0.0942 0.2937 0.062 Uiso 1 1 calc R . .
C23 C 0.2086(4) 0.1569(2) 0.23707(17) 0.0513(10) Uani 1 1 d . . .
C24 C 0.1476(5) 0.1055(2) 0.20032(19) 0.0666(12) Uani 1 1 d . . .
H24 H 0.1732 0.0610 0.2094 0.080 Uiso 1 1 calc R . .
C25 C 0.0535(5) 0.1186(2) 0.1525(2) 0.0712(13) Uani 1 1 d . . .
H25 H 0.0143 0.0838 0.1279 0.085 Uiso 1 1 calc R . .
C26 C 0.0148(5) 0.1841(2) 0.13992(19) 0.0659(12) Uani 1 1 d . . .
H26 H -0.0522 0.1932 0.1067 0.079 Uiso 1 1 calc R . .
C27 C 0.0705(4) 0.2354(2) 0.17402(18) 0.0553(10) Uani 1 1 d . . .
C28 C 0.1725(4) 0.2231(2) 0.22516(16) 0.0494(9) Uani 1 1 d . . .
C29 C 0.4532(4) 0.14676(19) 0.37397(17) 0.0513(9) Uani 1 1 d . . .
C30 C 0.6048(4) 0.1353(2) 0.36564(19) 0.0588(10) Uani 1 1 d . . .
C31 C 0.6787(5) 0.0982(2) 0.4106(2) 0.0669(12) Uani 1 1 d . . .
H31 H 0.7815 0.0885 0.4059 0.080 Uiso 1 1 calc R . .
C32 C 0.6065(5) 0.0752(2) 0.4617(2) 0.0684(12) Uani 1 1 d . . .
H32 H 0.6596 0.0499 0.4917 0.082 Uiso 1 1 calc R . .
C33 C 0.4586(5) 0.0885(2) 0.46951(18) 0.0611(11) Uani 1 1 d . . .
H33 H 0.4105 0.0731 0.5054 0.073 Uiso 1 1 calc R . .
C34 C 0.3774(4) 0.12424(19) 0.42590(17) 0.0526(10) Uani 1 1 d . . .
C35 C 0.2138(4) 0.1401(2) 0.43502(18) 0.0626(11) Uani 1 1 d . . .
H35 H 0.1670 0.1429 0.3930 0.075 Uiso 1 1 calc R . .
C36 C 0.1947(6) 0.2068(3) 0.4643(3) 0.1078(19) Uani 1 1 d . . .
H36A H 0.0890 0.2189 0.4634 0.162 Uiso 1 1 calc R . .
H36B H 0.2518 0.2397 0.4415 0.162 Uiso 1 1 calc R . .
H36C H 0.2309 0.2053 0.5071 0.162 Uiso 1 1 calc R . .
C37 C 0.1289(6) 0.0874(3) 0.4696(3) 0.1001(17) Uani 1 1 d . . .
H37A H 0.1676 0.0845 0.5120 0.150 Uiso 1 1 calc R . .
H37B H 0.1415 0.0447 0.4492 0.150 Uiso 1 1 calc R . .
H37C H 0.0228 0.0989 0.4701 0.150 Uiso 1 1 calc R . .
C38 C 0.6867(4) 0.1630(2) 0.3111(2) 0.0684(12) Uani 1 1 d . . .
H38 H 0.6269 0.2009 0.2945 0.082 Uiso 1 1 calc R . .
C39 C 0.8425(5) 0.1893(3) 0.3284(2) 0.1048(18) Uani 1 1 d . . .
H39A H 0.8356 0.2180 0.3645 0.157 Uiso 1 1 calc R . .
H39B H 0.8821 0.2145 0.2938 0.157 Uiso 1 1 calc R . .
H39C H 0.9090 0.1521 0.3378 0.157 Uiso 1 1 calc R . .
C40 C 0.6984(6) 0.1122(3) 0.2601(2) 0.0936(16) Uani 1 1 d . . .
H40A H 0.7555 0.0741 0.2751 0.140 Uiso 1 1 calc R . .
H40B H 0.7489 0.1319 0.2249 0.140 Uiso 1 1 calc R . .
H40C H 0.5982 0.0979 0.2474 0.140 Uiso 1 1 calc R . .
C41 C -0.0599(5) 0.3162(2) 0.1154(2) 0.0843(15) Uani 1 1 d . . .
H41A H -0.0193 0.2998 0.0767 0.126 Uiso 1 1 calc R . .
H41B H -0.0729 0.3641 0.1129 0.126 Uiso 1 1 calc R . .
H41C H -0.1566 0.2952 0.1226 0.126 Uiso 1 1 calc R . .
C1S C -0.378(2) 0.1025(7) 0.0518(12) 0.239(11) Uani 0.68(2) 1 d PD A 1
H1SA H -0.3588 0.0619 0.0759 0.287 Uiso 0.68(2) 1 calc PR A 1
H1SB H -0.4629 0.0926 0.0235 0.287 Uiso 0.68(2) 1 calc PR A 1
C1S' C -0.4242(14) 0.1254(9) 0.0304(5) 0.059(6) Uani 0.32(2) 1 d PD A 2
H1SC H -0.4751 0.0820 0.0305 0.071 Uiso 0.32(2) 1 calc PR A 2
H1SD H -0.4740 0.1535 -0.0010 0.071 Uiso 0.32(2) 1 calc PR A 2
Cl1S Cl -0.43957(18) 0.16248(9) 0.10331(7) 0.1214(6) Uani 1 1 d D . .
Cl2S Cl -0.23980(17) 0.11455(9) 0.01135(7) 0.1159(5) Uani 1 1 d D . .
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'
Cl Cl 0.1484 0.1585 '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
O1 Ni1 O3 178.45(12) . . ?
O1 Ni1 N1 93.37(12) . . ?
O3 Ni1 N1 86.87(12) . . ?
O1 Ni1 N2 86.68(12) . . ?
O3 Ni1 N2 93.14(12) . . ?
N1 Ni1 N2 178.04(12) . . ?
C2 N1 C9 114.2(3) . . ?
C2 N1 Ni1 124.5(3) . . ?
C9 N1 Ni1 121.2(2) . . ?
C22 N2 C29 113.1(3) . . ?
C22 N2 Ni1 125.3(3) . . ?
C29 N2 Ni1 121.6(2) . . ?
C8 O1 Ni1 129.8(2) . . ?
C7 O2 C21 116.6(3) . . ?
C28 O3 Ni1 129.1(2) . . ?
C27 O4 C41 116.2(3) . . ?
N1 C2 C3 127.2(4) . . ?
C8 C3 C2 120.5(4) . . ?
C8 C3 C4 119.9(4) . . ?
C2 C3 C4 119.6(4) . . ?
C5 C4 C3 121.4(4) . . ?
C4 C5 C6 119.6(4) . . ?
C7 C6 C5 121.3(4) . . ?
O2 C7 C6 126.3(4) . . ?
O2 C7 C8 113.9(4) . . ?
C6 C7 C8 119.9(4) . . ?
O1 C8 C3 124.4(3) . . ?
O1 C8 C7 117.7(4) . . ?
C3 C8 C7 117.9(4) . . ?
C10 C9 C14 122.4(4) . . ?
C10 C9 N1 119.4(4) . . ?
C14 C9 N1 118.2(3) . . ?
C11 C10 C9 118.0(4) . . ?
C11 C10 C18 120.5(4) . . ?
C9 C10 C18 121.5(4) . . ?
C12 C11 C10 121.0(5) . . ?
C11 C12 C13 120.7(4) . . ?
C12 C13 C14 121.5(5) . . ?
C13 C14 C9 116.3(4) . . ?
C13 C14 C15 120.9(4) . . ?
C9 C14 C15 122.8(4) . . ?
C14 C15 C17 112.1(4) . . ?
C14 C15 C16 112.1(4) . . ?
C17 C15 C16 110.1(5) . . ?
C10 C18 C20 113.3(5) . . ?
C10 C18 C19 111.1(4) . . ?
C20 C18 C19 110.5(5) . . ?
N2 C22 C23 126.6(4) . . ?
C28 C23 C24 120.8(4) . . ?
C28 C23 C22 120.6(4) . . ?
C24 C23 C22 118.6(4) . . ?
C25 C24 C23 121.2(4) . . ?
C24 C25 C26 119.2(4) . . ?
C27 C26 C25 121.9(4) . . ?
O4 C27 C26 126.3(4) . . ?
O4 C27 C28 113.4(4) . . ?
C26 C27 C28 120.3(4) . . ?
O3 C28 C23 125.0(3) . . ?
O3 C28 C27 118.4(4) . . ?
C23 C28 C27 116.6(4) . . ?
C30 C29 C34 122.5(3) . . ?
C30 C29 N2 118.5(3) . . ?
C34 C29 N2 118.9(3) . . ?
C31 C30 C29 117.0(4) . . ?
C31 C30 C38 121.2(4) . . ?
C29 C30 C38 121.8(4) . . ?
C32 C31 C30 121.6(4) . . ?
C33 C32 C31 120.3(4) . . ?
C32 C33 C34 121.2(4) . . ?
C33 C34 C29 117.5(4) . . ?
C33 C34 C35 121.2(4) . . ?
C29 C34 C35 121.2(3) . . ?
C36 C35 C37 111.2(4) . . ?
C36 C35 C34 111.2(4) . . ?
C37 C35 C34 114.2(4) . . ?
C30 C38 C40 111.2(4) . . ?
C30 C38 C39 112.8(4) . . ?
C40 C38 C39 109.9(4) . . ?
Cl2S C1S Cl1S 121.1(7) . . ?
Cl2S C1S' Cl1S 111.0(7) . . ?
C1S Cl1S C1S' 25.4(9) . . ?
C1S Cl2S C1S' 26.5(10) . . ?
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 O1 1.827(3) . ?
Ni1 O3 1.834(3) . ?
Ni1 N1 1.907(3) . ?
Ni1 N2 1.908(3) . ?
N1 C2 1.300(4) . ?
N1 C9 1.459(4) . ?
N2 C22 1.289(4) . ?
N2 C29 1.467(4) . ?
O1 C8 1.293(4) . ?
O2 C7 1.348(5) . ?
O2 C21 1.433(4) . ?
O3 C28 1.288(4) . ?
O4 C27 1.360(5) . ?
O4 C41 1.430(4) . ?
C2 C3 1.412(5) . ?
C3 C8 1.401(6) . ?
C3 C4 1.421(5) . ?
C4 C5 1.362(5) . ?
C5 C6 1.399(6) . ?
C6 C7 1.380(6) . ?
C7 C8 1.450(5) . ?
C9 C10 1.391(5) . ?
C9 C14 1.410(5) . ?
C10 C11 1.386(6) . ?
C10 C18 1.509(6) . ?
C11 C12 1.368(7) . ?
C12 C13 1.368(7) . ?
C13 C14 1.401(6) . ?
C14 C15 1.496(6) . ?
C15 C17 1.519(7) . ?
C15 C16 1.521(6) . ?
C18 C20 1.515(7) . ?
C18 C19 1.529(7) . ?
C22 C23 1.412(5) . ?
C23 C28 1.403(5) . ?
C23 C24 1.416(5) . ?
C24 C25 1.354(5) . ?
C25 C26 1.396(6) . ?
C26 C27 1.367(6) . ?
C27 C28 1.450(5) . ?
C29 C30 1.395(5) . ?
C29 C34 1.403(5) . ?
C30 C31 1.393(5) . ?
C30 C38 1.512(6) . ?
C31 C32 1.374(6) . ?
C32 C33 1.368(6) . ?
C33 C34 1.389(5) . ?
C34 C35 1.519(5) . ?
C35 C36 1.505(6) . ?
C35 C37 1.518(6) . ?
C38 C40 1.515(6) . ?
C38 C39 1.538(6) . ?
C1S Cl2S 1.553(12) . ?
C1S Cl1S 1.746(11) . ?
C1S' Cl2S 1.726(12) . ?
C1S' Cl1S 1.761(10) . ?
