#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:34:00 +0100 (vie 25 de mar de 2016) $
#$Revision: 179796 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009252.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_7009252
loop_
_publ_author_name
'De-qiang Ma'
'Shiro Hikichi'
'Munetaka Akita'
'Yoshihiko Moro-oka'
_publ_section_title
;
 An entry to half-sandwich complexes of first row transition metals
 (Ni, Co, Mn) containing the Kläui tripodal ligand, LOMe: synthesis
 and crystal structures of oligomeric, [LOMeM(μ-X)(L)]n
 (n = 2, 4), and monomeric complexes, LOMeM(L2)(X)
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1123
_journal_page_last               1134
_journal_paper_doi               10.1039/a909580b
_journal_year                    2000
_chemical_formula_sum            'C36 H58 Cl4 Co2 N2 Ni2 O24 P6'
_chemical_formula_weight         1465.74
_chemical_name_common            'compound 7c(Ni)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.374(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.196(4)
_cell_length_b                   24.838(3)
_cell_length_c                   10.667(2)
_cell_measurement_temperature    213(2)
_cell_volume                     6305.9(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.765
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5546
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.497
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2992
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.799
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.799
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          1.019
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                5164
_reflns_number_total             5546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909580b.txt
_cod_data_source_block           7c
_cod_original_cell_volume        6305.9(17)
_cod_database_code               7009252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.21612(2) 0.29373(2) 0.05770(6) 0.0216(2) Uani 1 1 d . . .
Co1 Co 0.09647(3) 0.39614(3) 0.04059(7) 0.0253(2) Uani 1 1 d . . .
Cl1 Cl 0.1486(2) 0.0663(2) 0.6310(5) 0.1451(17) Uani 1 1 d . . .
Cl2 Cl 0.0773(3) 0.1438(3) 0.7251(9) 0.248(5) Uani 1 1 d . . .
P1 P 0.12101(5) 0.35950(6) -0.12540(12) 0.0258(3) Uani 1 1 d . . .
P2 P 0.18396(6) 0.41224(6) 0.12175(14) 0.0289(3) Uani 1 1 d . . .
P3 P 0.09784(5) 0.31824(5) 0.13021(12) 0.0249(3) Uani 1 1 d . . .
O11 O 0.16760(15) 0.31901(14) -0.1080(3) 0.0258(7) Uani 1 1 d . . .
O12 O 0.06605(17) 0.3334(2) -0.2064(4) 0.0460(11) Uani 1 1 d . . .
O13 O 0.1330(2) 0.4037(2) -0.2265(4) 0.0470(12) Uani 1 1 d . . .
O21 O 0.22874(16) 0.37121(15) 0.1154(4) 0.0319(8) Uani 1 1 d . . .
O22 O 0.19993(18) 0.46693(17) 0.0583(5) 0.0418(10) Uani 1 1 d . . .
O23 O 0.1904(2) 0.4329(2) 0.2660(4) 0.0471(11) Uani 1 1 d . . .
O31 O 0.15135(15) 0.28675(15) 0.1524(3) 0.0278(8) Uani 1 1 d . . .
O32 O 0.07730(18) 0.32513(18) 0.2641(4) 0.0379(9) Uani 1 1 d . . .
O33 O 0.04846(17) 0.28050(17) 0.0563(4) 0.0380(9) Uani 1 1 d . . .
O51 O 0.21450(14) 0.21255(14) 0.0270(4) 0.0253(7) Uani 1 1 d . . .
O52 O 0.26901(17) 0.27066(18) 0.2295(4) 0.0372(9) Uani 1 1 d . . .
O53 O 0.2898(3) 0.2273(3) 0.4038(5) 0.0755(19) Uani 1 1 d . . .
N1 N 0.2621(2) 0.2315(2) 0.2962(5) 0.0427(13) Uani 1 1 d . . .
C12 C 0.0717(4) 0.3034(5) -0.3186(8) 0.077(3) Uani 1 1 d . . .
H1 H 0.0362 0.2877 -0.3549 0.077 Uiso 1 1 calc R . .
H2 H 0.0990 0.2754 -0.2962 0.077 Uiso 1 1 calc R . .
H3 H 0.0838 0.3270 -0.3796 0.077 Uiso 1 1 calc R . .
C13 C 0.1876(4) 0.4222(3) -0.2334(8) 0.058(2) Uani 1 1 d . . .
H4 H 0.2147 0.4017 -0.1760 0.058 Uiso 1 1 calc R . .
H5 H 0.1908 0.4596 -0.2101 0.058 Uiso 1 1 calc R . .
H6 H 0.1943 0.4180 -0.3189 0.058 Uiso 1 1 calc R . .
C22 C 0.2578(3) 0.4828(3) 0.0748(10) 0.068(2) Uani 1 1 d . . .
H7 H 0.2802 0.4526 0.0583 0.068 Uiso 1 1 calc R . .
H8 H 0.2702 0.4951 0.1606 0.068 Uiso 1 1 calc R . .
H9 H 0.2618 0.5114 0.0164 0.068 Uiso 1 1 calc R . .
C23 C 0.1960(5) 0.3945(4) 0.3677(7) 0.073(3) Uani 1 1 d . . .
H10 H 0.1832 0.3599 0.3342 0.073 Uiso 1 1 calc R . .
H11 H 0.1738 0.4058 0.4291 0.073 Uiso 1 1 calc R . .
H12 H 0.2347 0.3920 0.4080 0.073 Uiso 1 1 calc R . .
C32 C 0.0806(3) 0.2791(3) 0.3455(7) 0.0551(19) Uani 1 1 d . . .
H13 H 0.0555 0.2836 0.4048 0.055 Uiso 1 1 calc R . .
H14 H 0.1183 0.2752 0.3913 0.055 Uiso 1 1 calc R . .
H15 H 0.0702 0.2475 0.2949 0.055 Uiso 1 1 calc R . .
C33 C 0.0607(3) 0.2310(3) -0.0009(10) 0.067(2) Uani 1 1 d . . .
H16 H 0.0323 0.2239 -0.0741 0.067 Uiso 1 1 calc R . .
H17 H 0.0615 0.2023 0.0596 0.067 Uiso 1 1 calc R . .
H18 H 0.0967 0.2336 -0.0266 0.067 Uiso 1 1 calc R . .
C41 C 0.0572(4) 0.4626(3) -0.0538(8) 0.063(3) Uani 1 1 d . . .
C42 C 0.0167(3) 0.4196(3) -0.0555(6) 0.0432(15) Uani 1 1 d . . .
C43 C 0.0150(2) 0.4071(3) 0.0718(7) 0.0394(14) Uani 1 1 d . . .
C44 C 0.0513(3) 0.4409(3) 0.1522(6) 0.0404(14) Uani 1 1 d . . .
C45 C 0.0777(3) 0.4762(2) 0.0733(8) 0.0495(18) Uani 1 1 d . . .
C51 C 0.2033(2) 0.1815(2) 0.1169(6) 0.0332(12) Uani 1 1 d . . .
C52 C 0.2223(3) 0.1905(3) 0.2495(6) 0.0410(15) Uani 1 1 d . . .
C53 C 0.2046(3) 0.1570(3) 0.3415(8) 0.061(2) Uani 1 1 d . . .
C54 C 0.1699(4) 0.1156(4) 0.3077(11) 0.077(3) Uani 1 1 d . . .
C55 C 0.1526(4) 0.1035(3) 0.1763(11) 0.069(3) Uani 1 1 d . . .
C56 C 0.1692(3) 0.1359(3) 0.0867(8) 0.0495(17) Uani 1 1 d . . .
C61 C 0.1454(6) 0.1324(7) 0.6843(16) 0.126(5) Uani 1 1 d . . .
H19 H 0.0663 0.4790 -0.1276 0.074 Uiso 1 1 d . . .
H20 H -0.0046 0.4032 -0.1298 0.053 Uiso 1 1 d . . .
H21 H -0.0079 0.3796 0.0988 0.047 Uiso 1 1 d . . .
H22 H 0.0576 0.4415 0.2436 0.048 Uiso 1 1 d . . .
H23 H 0.1040 0.5041 0.1022 0.061 Uiso 1 1 d . . .
H24 H 0.2170 0.1647 0.4312 0.075 Uiso 1 1 d . . .
H25 H 0.1579 0.0941 0.3712 0.091 Uiso 1 1 d . . .
H26 H 0.1302 0.0727 0.1502 0.084 Uiso 1 1 d . . .
H27 H 0.1562 0.1276 -0.0015 0.062 Uiso 1 1 d . . .
H28 H 0.1754 0.1385 0.7533 0.158 Uiso 1 1 d . . .
H29 H 0.1517 0.1561 0.6144 0.158 Uiso 1 1 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'
P P 0.1023 0.0942 '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 0.3494 0.9721 '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
O31 Ni1 O21 91.02(16) . . ?
O31 Ni1 O11 94.73(14) . . ?
O21 Ni1 O11 90.14(15) . . ?
O31 Ni1 O51 90.08(14) . . ?
O21 Ni1 O51 169.67(15) . . ?
O11 Ni1 O51 100.01(15) . . ?
O31 Ni1 O51 169.95(15) . 7 ?
O21 Ni1 O51 96.62(15) . 7 ?
O11 Ni1 O51 91.77(14) . 7 ?
O51 Ni1 O51 81.24(15) . 7 ?
O31 Ni1 O52 86.92(16) . . ?
O21 Ni1 O52 87.69(17) . . ?
O11 Ni1 O52 177.29(17) . . ?
O51 Ni1 O52 82.11(16) . . ?
O51 Ni1 O52 86.88(16) 7 . ?
C41 Co1 C43 66.9(3) . . ?
C41 Co1 C44 67.0(3) . . ?
C43 Co1 C44 39.2(3) . . ?
C41 Co1 C45 39.3(3) . . ?
C43 Co1 C45 66.8(3) . . ?
C44 Co1 C45 40.6(3) . . ?
C41 Co1 C42 40.6(4) . . ?
C43 Co1 C42 39.2(3) . . ?
C44 Co1 C42 66.3(3) . . ?
C45 Co1 C42 66.9(3) . . ?
C41 Co1 P3 154.1(3) . . ?
C43 Co1 P3 89.20(18) . . ?
C44 Co1 P3 101.18(19) . . ?
C45 Co1 P3 140.3(2) . . ?
C42 Co1 P3 113.9(2) . . ?
C41 Co1 P1 96.1(2) . . ?
C43 Co1 P1 126.5(2) . . ?
C44 Co1 P1 160.54(19) . . ?
C45 Co1 P1 129.6(2) . . ?
C42 Co1 P1 94.64(18) . . ?
P3 Co1 P1 90.04(6) . . ?
C41 Co1 P2 112.0(3) . . ?
C43 Co1 P2 142.8(2) . . ?
C44 Co1 P2 104.4(2) . . ?
C45 Co1 P2 89.0(2) . . ?
C42 Co1 P2 152.5(2) . . ?
P3 Co1 P2 93.00(6) . . ?
P1 Co1 P2 90.70(6) . . ?
O11 P1 O12 109.4(2) . . ?
O11 P1 O13 108.7(2) . . ?
O12 P1 O13 98.5(3) . . ?
O11 P1 Co1 119.45(15) . . ?
O12 P1 Co1 106.87(17) . . ?
O13 P1 Co1 111.8(2) . . ?
O21 P2 O22 109.1(2) . . ?
O21 P2 O23 108.4(2) . . ?
O22 P2 O23 98.4(3) . . ?
O21 P2 Co1 121.13(16) . . ?
O22 P2 Co1 106.28(18) . . ?
O23 P2 Co1 111.1(2) . . ?
O31 P3 O32 108.3(2) . . ?
O31 P3 O33 108.6(2) . . ?
O32 P3 O33 100.2(2) . . ?
O31 P3 Co1 118.93(16) . . ?
O32 P3 Co1 108.46(17) . . ?
O33 P3 Co1 110.78(17) . . ?
P1 O11 Ni1 128.2(2) . . ?
C12 O12 P1 117.9(4) . . ?
C13 O13 P1 122.8(4) . . ?
P2 O21 Ni1 126.1(2) . . ?
C22 O22 P2 119.2(5) . . ?
C23 O23 P2 119.6(5) . . ?
P3 O31 Ni1 127.2(2) . . ?
C32 O32 P3 117.6(4) . . ?
C33 O33 P3 121.2(4) . . ?
C51 O51 Ni1 118.0(3) . . ?
C51 O51 Ni1 125.2(3) . 7 ?
Ni1 O51 Ni1 98.76(15) . 7 ?
N1 O52 Ni1 126.1(4) . . ?
O53 N1 O52 119.9(7) . . ?
O53 N1 C52 119.2(6) . . ?
O52 N1 C52 120.9(5) . . ?
C45 C41 C42 108.2(6) . . ?
C45 C41 Co1 70.7(4) . . ?
C42 C41 Co1 70.6(4) . . ?
C43 C42 C41 106.8(6) . . ?
C43 C42 Co1 69.5(3) . . ?
C41 C42 Co1 68.8(4) . . ?
C44 C43 C42 109.8(6) . . ?
C44 C43 Co1 70.6(3) . . ?
C42 C43 Co1 71.3(3) . . ?
C43 C44 C45 107.7(6) . . ?
C43 C44 Co1 70.3(3) . . ?
C45 C44 Co1 69.9(3) . . ?
C41 C45 C44 107.5(6) . . ?
C41 C45 Co1 70.0(4) . . ?
C44 C45 Co1 69.6(3) . . ?
O51 C51 C56 120.1(6) . . ?
O51 C51 C52 124.6(5) . . ?
C56 C51 C52 115.3(6) . . ?
C53 C52 C51 120.8(7) . . ?
C53 C52 N1 116.7(7) . . ?
C51 C52 N1 122.4(5) . . ?
C54 C53 C52 121.4(9) . . ?
C53 C54 C55 119.3(7) . . ?
C56 C55 C54 119.6(8) . . ?
C55 C56 C51 123.4(8) . . ?
Cl1 C61 Cl2 108.9(8) . . ?
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 O31 2.019(3) . ?
Ni1 O21 2.027(4) . ?
Ni1 O11 2.037(4) . ?
Ni1 O51 2.042(4) . ?
Ni1 O51 2.050(3) 7 ?
Ni1 O52 2.117(4) . ?
Co1 C41 2.074(6) . ?
Co1 C43 2.075(5) . ?
Co1 C44 2.079(5) . ?
Co1 C45 2.083(6) . ?
Co1 C42 2.098(6) . ?
Co1 P3 2.1558(15) . ?
Co1 P1 2.1668(14) . ?
Co1 P2 2.1749(16) . ?
Cl1 C61 1.743(18) . ?
Cl2 C61 1.800(18) . ?
P1 O11 1.497(4) . ?
P1 O12 1.587(5) . ?
P1 O13 1.602(4) . ?
P2 O21 1.498(4) . ?
P2 O22 1.596(4) . ?
P2 O23 1.603(5) . ?
P3 O31 1.495(4) . ?
P3 O32 1.604(4) . ?
P3 O33 1.609(4) . ?
O12 C12 1.438(8) . ?
O13 C13 1.414(9) . ?
O22 C22 1.435(9) . ?
O23 C23 1.432(10) . ?
O32 C32 1.429(8) . ?
O33 C33 1.426(8) . ?
O51 C51 1.297(7) . ?
O51 Ni1 2.050(3) 7 ?
O52 N1 1.234(7) . ?
O53 N1 1.225(8) . ?
N1 C52 1.427(10) . ?
C41 C45 1.399(12) . ?
C41 C42 1.446(12) . ?
C42 C43 1.401(9) . ?
C43 C44 1.392(10) . ?
C44 C45 1.442(9) . ?
C51 C56 1.404(9) . ?
C51 C52 1.425(9) . ?
C52 C53 1.412(9) . ?
C53 C54 1.334(15) . ?
C54 C55 1.421(15) . ?
C55 C56 1.365(11) . ?
