#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:42 +0100 (vie 25 de mar de 2016) $
#$Revision: 179801 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/97/7009708.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_7009708
loop_
_publ_author_name
'Kimblin, Clare'
'Bridgewater, Brian M.'
'Churchill, David G.'
'Parkin, Gerard'
_publ_section_title
;
 Synthesis and molecular structures of a pair of
 tris(imidazolyl)phosphine cobalt--perchlorate complexes,
 {[PimPri2]Co(OClO3)}[ClO4] and {[PimPri2]Co(OH2)(HOMe)(OClO3)}[ClO4]
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2191
_journal_paper_doi               10.1039/b002894k
_journal_year                    2000
_chemical_formula_sum            'C29 H47 Cl8 Co N6 O8 P'
_chemical_formula_weight         981.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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                 100.1540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3832(11)
_cell_length_b                   16.8991(12)
_cell_length_c                   17.8228(11)
_cell_measurement_temperature    238(2)
_cell_volume                     4560.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      238(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31912
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_T_min  0.7681
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         10147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1135P)²+1.5503P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                6201
_reflns_number_total             10147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002894k.txt
_cod_data_source_block           cobs10
_cod_database_code               7009708
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
Co Co 0.12016(3) 0.16088(3) 0.15856(3) 0.04290(17) Uani 1 1 d . . .
N11 N 0.3878(2) 0.1811(2) 0.1806(2) 0.0599(9) Uani 1 1 d . . .
N12 N 0.2447(2) 0.20362(19) 0.17058(16) 0.0478(7) Uani 1 1 d . . .
N21 N 0.1979(2) 0.02183(19) -0.00577(15) 0.0475(7) Uani 1 1 d . . .
N22 N 0.12734(19) 0.10369(17) 0.05948(15) 0.0417(7) Uani 1 1 d . . .
N31 N 0.2374(2) -0.03284(19) 0.26982(17) 0.0495(8) Uani 1 1 d . . .
N32 N 0.1486(2) 0.06651(17) 0.22838(15) 0.0425(7) Uani 1 1 d . . .
C11 C 0.3060(3) 0.1483(2) 0.1654(2) 0.0494(9) Uani 1 1 d . . .
C12 C 0.3765(3) 0.2597(3) 0.1947(3) 0.0669(12) Uani 1 1 d . . .
H12A H 0.4219 0.2973 0.2066 0.080 Uiso 1 1 calc R . .
C13 C 0.2886(3) 0.2741(2) 0.1888(2) 0.0552(10) Uani 1 1 d . . .
C14 C 0.4730(3) 0.1387(4) 0.1804(4) 0.0916(17) Uani 1 1 d . . .
H14A H 0.4538 0.0876 0.1558 0.110 Uiso 1 1 calc R . .
C15 C 0.5146(6) 0.1158(7) 0.2548(5) 0.188(5) Uani 1 1 d . . .
H15A H 0.4719 0.0897 0.2805 0.282 Uiso 1 1 calc R . .
H15B H 0.5375 0.1623 0.2835 0.282 Uiso 1 1 calc R . .
H15C H 0.5627 0.0797 0.2512 0.282 Uiso 1 1 calc R . .
C16 C 0.5220(6) 0.1755(6) 0.1264(7) 0.181(5) Uani 1 1 d . . .
H16A H 0.4893 0.1692 0.0750 0.272 Uiso 1 1 calc R . .
H16B H 0.5793 0.1502 0.1303 0.272 Uiso 1 1 calc R . .
H16C H 0.5301 0.2313 0.1380 0.272 Uiso 1 1 calc R . .
C17 C 0.2409(3) 0.3500(3) 0.1969(3) 0.0665(12) Uani 1 1 d . . .
H17A H 0.2040 0.3432 0.2366 0.080 Uiso 1 1 calc R . .
C18 C 0.1812(4) 0.3724(3) 0.1220(4) 0.0917(17) Uani 1 1 d . . .
H18A H 0.1366 0.3318 0.1084 0.138 Uiso 1 1 calc R . .
H18B H 0.2164 0.3769 0.0821 0.138 Uiso 1 1 calc R . .
H18C H 0.1528 0.4227 0.1280 0.138 Uiso 1 1 calc R . .
C19 C 0.3074(4) 0.4176(3) 0.2212(4) 0.1001(19) Uani 1 1 d . . .
H19A H 0.3450 0.4039 0.2690 0.150 Uiso 1 1 calc R . .
H19B H 0.2756 0.4660 0.2277 0.150 Uiso 1 1 calc R . .
H19C H 0.3434 0.4254 0.1823 0.150 Uiso 1 1 calc R . .
C21 C 0.1984(2) 0.0562(2) 0.06216(18) 0.0445(8) Uani 1 1 d . . .
C22 C 0.1228(3) 0.0482(2) -0.0544(2) 0.0537(10) Uani 1 1 d . . .
H22A H 0.1050 0.0343 -0.1058 0.064 Uiso 1 1 calc R . .
C23 C 0.0799(2) 0.0983(2) -0.01330(19) 0.0457(8) Uani 1 1 d . . .
C24 C 0.2666(3) -0.0307(3) -0.0272(2) 0.0585(10) Uani 1 1 d . . .
H24A H 0.2999 -0.0525 0.0210 0.070 Uiso 1 1 calc R . .
C25 C 0.3315(5) 0.0162(4) -0.0627(5) 0.132(3) Uani 1 1 d . . .
H25A H 0.3825 -0.0164 -0.0663 0.197 Uiso 1 1 calc R . .
H25B H 0.3501 0.0623 -0.0315 0.197 Uiso 1 1 calc R . .
H25C H 0.3038 0.0331 -0.1133 0.197 Uiso 1 1 calc R . .
C26 C 0.2262(4) -0.0995(4) -0.0726(5) 0.121(3) Uani 1 1 d . . .
H26A H 0.2724 -0.1348 -0.0830 0.181 Uiso 1 1 calc R . .
H26B H 0.1921 -0.0809 -0.1203 0.181 Uiso 1 1 calc R . .
H26C H 0.1877 -0.1277 -0.0441 0.181 Uiso 1 1 calc R . .
C27 C -0.0018(3) 0.1472(2) -0.0395(2) 0.0526(10) Uani 1 1 d . . .
H27A H -0.0367 0.1475 0.0022 0.063 Uiso 1 1 calc R . .
C28 C -0.0593(3) 0.1117(3) -0.1097(3) 0.0762(14) Uani 1 1 d . . .
H28A H -0.1124 0.1433 -0.1235 0.114 Uiso 1 1 calc R . .
H28B H -0.0753 0.0580 -0.0988 0.114 Uiso 1 1 calc R . .
H28C H -0.0268 0.1114 -0.1517 0.114 Uiso 1 1 calc R . .
C29 C 0.0232(3) 0.2321(3) -0.0534(3) 0.0730(13) Uani 1 1 d . . .
H29A H 0.0541 0.2549 -0.0062 0.110 Uiso 1 1 calc R . .
H29B H -0.0299 0.2625 -0.0715 0.110 Uiso 1 1 calc R . .
H29C H 0.0612 0.2332 -0.0914 0.110 Uiso 1 1 calc R . .
C31 C 0.2188(2) 0.0243(2) 0.21686(18) 0.0426(8) Uani 1 1 d . . .
C32 C 0.1760(3) -0.0271(2) 0.3169(2) 0.0538(10) Uani 1 1 d . . .
H32A H 0.1728 -0.0596 0.3592 0.065 Uiso 1 1 calc R . .
C33 C 0.1206(3) 0.0340(2) 0.29173(19) 0.0463(8) Uani 1 1 d . . .
C34 C 0.3107(3) -0.0906(3) 0.2784(2) 0.0587(10) Uani 1 1 d . . .
H34A H 0.3382 -0.0869 0.2323 0.070 Uiso 1 1 calc R . .
C35 C 0.3802(4) -0.0693(4) 0.3459(4) 0.104(2) Uani 1 1 d . . .
H35A H 0.3991 -0.0151 0.3408 0.155 Uiso 1 1 calc R . .
H35B H 0.4304 -0.1045 0.3481 0.155 Uiso 1 1 calc R . .
H35C H 0.3559 -0.0746 0.3923 0.155 Uiso 1 1 calc R . .
C36 C 0.2763(4) -0.1731(3) 0.2820(4) 0.0938(18) Uani 1 1 d . . .
H36A H 0.2278 -0.1816 0.2399 0.141 Uiso 1 1 calc R . .
H36B H 0.2555 -0.1806 0.3299 0.141 Uiso 1 1 calc R . .
H36C H 0.3231 -0.2107 0.2786 0.141 Uiso 1 1 calc R . .
C37 C 0.0412(3) 0.0636(3) 0.3208(2) 0.0553(10) Uani 1 1 d . . .
H37A H 0.0421 0.1222 0.3200 0.066 Uiso 1 1 calc R . .
C38 C -0.0432(3) 0.0352(3) 0.2682(3) 0.0765(14) Uani 1 1 d . . .
H38A H -0.0434 0.0542 0.2168 0.115 Uiso 1 1 calc R . .
H38B H -0.0945 0.0556 0.2866 0.115 Uiso 1 1 calc R . .
H38C H -0.0449 -0.0222 0.2681 0.115 Uiso 1 1 calc R . .
C39 C 0.0416(4) 0.0365(3) 0.4029(3) 0.0826(15) Uani 1 1 d . . .
H39A H 0.0932 0.0578 0.4359 0.124 Uiso 1 1 calc R . .
H39B H 0.0433 -0.0208 0.4051 0.124 Uiso 1 1 calc R . .
H39C H -0.0113 0.0553 0.4197 0.124 Uiso 1 1 calc R . .
P P 0.28644(6) 0.04368(6) 0.14425(5) 0.0448(2) Uani 1 1 d . . .
Cl1 Cl -0.01533(9) 0.25644(7) 0.19881(7) 0.0710(3) Uani 1 1 d . . .
O11 O -0.0015(2) 0.2066(2) 0.13621(19) 0.0829(10) Uani 1 1 d . . .
O12 O -0.0354(3) 0.3337(2) 0.1712(3) 0.1200(16) Uani 1 1 d . . .
O13 O -0.0835(3) 0.2256(2) 0.2350(2) 0.0975(12) Uani 1 1 d . . .
O14 O 0.0681(3) 0.2539(2) 0.2505(2) 0.0930(11) Uani 1 1 d . . .
Cl2 Cl 0.44686(11) -0.15782(11) 0.11572(10) 0.0987(5) Uani 1 1 d . . .
O21 O 0.4822(8) -0.2276(8) 0.1135(8) 0.346(8) Uani 1 1 d . . .
O22 O 0.4666(5) -0.1032(7) 0.0672(6) 0.277(6) Uani 1 1 d . . .
O23 O 0.4713(4) -0.1329(6) 0.1924(4) 0.206(4) Uani 1 1 d . . .
O24 O 0.3530(3) -0.1627(3) 0.1048(3) 0.1168(15) Uani 1 1 d . . .
C1 C -0.2722(5) 0.1609(4) 0.4326(3) 0.0953(18) Uani 1 1 d . . .
H1A H -0.3173 0.2033 0.4260 0.114 Uiso 1 1 calc R . .
Cl11 Cl -0.3226(2) 0.07141(16) 0.44759(14) 0.1733(11) Uani 1 1 d . . .
Cl12 Cl -0.19039(17) 0.18397(14) 0.51065(11) 0.1377(8) Uani 1 1 d . . .
Cl13 Cl -0.22644(15) 0.15441(12) 0.34983(10) 0.1244(7) Uani 1 1 d . . .
C2 C 0.6457(4) -0.2025(3) 0.5593(3) 0.0814(15) Uani 1 1 d . . .
H2A H 0.5996 -0.2347 0.5771 0.098 Uiso 1 1 calc R . .
Cl21 Cl 0.59457(18) -0.13128(14) 0.49680(13) 0.1472(8) Uani 1 1 d . . .
Cl22 Cl 0.70986(19) -0.15951(15) 0.63700(13) 0.1649(10) Uani 1 1 d . . .
Cl23 Cl 0.70977(14) -0.26551(11) 0.51132(10) 0.1165(6) Uani 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'
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
O11 Co N32 121.41(14) . . ?
O11 Co N12 135.97(16) . . ?
N32 Co N12 96.77(12) . . ?
O11 Co N22 101.71(13) . . ?
N32 Co N22 96.92(11) . . ?
N12 Co N22 93.79(12) . . ?
O11 Co O14 59.42(14) . . ?
N32 Co O14 98.76(12) . . ?
N12 Co O14 96.47(13) . . ?
N22 Co O14 160.08(12) . . ?
C11 N11 C12 106.9(4) . . ?
C11 N11 C14 125.9(4) . . ?
C12 N11 C14 127.2(4) . . ?
C11 N12 C13 107.3(3) . . ?
C11 N12 Co 114.0(3) . . ?
C13 N12 Co 138.4(3) . . ?
C21 N21 C22 107.2(3) . . ?
C21 N21 C24 126.9(3) . . ?
C22 N21 C24 125.8(3) . . ?
C21 N22 C23 106.6(3) . . ?
C21 N22 Co 114.8(2) . . ?
C23 N22 Co 138.6(3) . . ?
C31 N31 C32 107.1(3) . . ?
C31 N31 C34 127.6(3) . . ?
C32 N31 C34 125.3(3) . . ?
C31 N32 C33 106.7(3) . . ?
C31 N32 Co 114.8(2) . . ?
C33 N32 Co 138.2(2) . . ?
N12 C11 N11 109.8(3) . . ?
N12 C11 P 126.7(3) . . ?
N11 C11 P 123.4(3) . . ?
C13 C12 N11 108.4(4) . . ?
C12 C13 N12 107.6(4) . . ?
C12 C13 C17 130.0(4) . . ?
N12 C13 C17 122.3(4) . . ?
C15 C14 C16 122.0(7) . . ?
C15 C14 N11 112.3(6) . . ?
C16 C14 N11 110.7(6) . . ?
C13 C17 C18 110.9(4) . . ?
C13 C17 C19 110.5(4) . . ?
C18 C17 C19 109.2(4) . . ?
N21 C21 N22 110.4(3) . . ?
N21 C21 P 124.0(3) . . ?
N22 C21 P 125.5(3) . . ?
C23 C22 N21 107.0(3) . . ?
C22 C23 N22 108.7(3) . . ?
C22 C23 C27 129.1(3) . . ?
N22 C23 C27 122.0(3) . . ?
N21 C24 C26 111.0(4) . . ?
N21 C24 C25 110.5(4) . . ?
C26 C24 C25 115.4(5) . . ?
C23 C27 C29 110.4(3) . . ?
C23 C27 C28 111.7(4) . . ?
C29 C27 C28 111.4(4) . . ?
N32 C31 N31 110.6(3) . . ?
N32 C31 P 126.0(3) . . ?
N31 C31 P 123.3(3) . . ?
C33 C32 N31 108.0(3) . . ?
C32 C33 N32 107.5(3) . . ?
C32 C33 C37 129.9(3) . . ?
N32 C33 C37 122.6(3) . . ?
N31 C34 C36 110.5(4) . . ?
N31 C34 C35 110.2(4) . . ?
C36 C34 C35 113.3(5) . . ?
C33 C37 C39 111.4(4) . . ?
C33 C37 C38 109.7(3) . . ?
C39 C37 C38 110.5(4) . . ?
C11 P C21 97.21(17) . . ?
C11 P C31 96.98(17) . . ?
C21 P C31 98.87(16) . . ?
O12 Cl1 O13 111.3(3) . . ?
O12 Cl1 O14 111.4(3) . . ?
O13 Cl1 O14 110.1(3) . . ?
O12 Cl1 O11 108.9(3) . . ?
O13 Cl1 O11 110.9(2) . . ?
O14 Cl1 O11 103.9(2) . . ?
Cl1 O11 Co 109.40(19) . . ?
Cl1 O14 Co 87.24(17) . . ?
O21 Cl2 O22 117.5(8) . . ?
O21 Cl2 O23 104.9(7) . . ?
O22 Cl2 O23 111.5(7) . . ?
O21 Cl2 O24 111.2(7) . . ?
O22 Cl2 O24 107.0(4) . . ?
O23 Cl2 O24 103.8(4) . . ?
Cl11 C1 Cl13 109.4(4) . . ?
Cl11 C1 Cl12 110.4(3) . . ?
Cl13 C1 Cl12 110.2(4) . . ?
Cl22 C2 Cl21 110.9(3) . . ?
Cl22 C2 Cl23 110.8(3) . . ?
Cl21 C2 Cl23 109.6(3) . . ?
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
Co O11 1.999(3) . ?
Co N32 2.023(3) . ?
Co N12 2.024(3) . ?
Co N22 2.033(3) . ?
Co O14 2.502(4) . ?
N11 C11 1.358(5) . ?
N11 C12 1.369(6) . ?
N11 C14 1.493(6) . ?
N12 C11 1.343(5) . ?
N12 C13 1.379(5) . ?
N21 C21 1.342(4) . ?
N21 C22 1.389(5) . ?
N21 C24 1.482(5) . ?
N22 C21 1.350(5) . ?
N22 C23 1.375(4) . ?
N31 C31 1.345(4) . ?
N31 C32 1.372(5) . ?
N31 C34 1.480(5) . ?
N32 C31 1.339(5) . ?
N32 C33 1.391(4) . ?
C11 P 1.821(4) . ?
C12 C13 1.360(6) . ?
C13 C17 1.499(6) . ?
C14 C15 1.421(10) . ?
C14 C16 1.463(11) . ?
C17 C18 1.528(7) . ?
C17 C19 1.543(7) . ?
C21 P 1.822(4) . ?
C22 C23 1.363(5) . ?
C23 C27 1.508(5) . ?
C24 C26 1.489(7) . ?
C24 C25 1.500(8) . ?
C27 C29 1.517(6) . ?
C27 C28 1.523(6) . ?
C31 P 1.828(4) . ?
C32 C33 1.364(5) . ?
C33 C37 1.494(5) . ?
C34 C36 1.497(7) . ?
C34 C35 1.506(7) . ?
C37 C39 1.533(6) . ?
C37 C38 1.538(7) . ?
Cl1 O12 1.410(4) . ?
Cl1 O13 1.424(4) . ?
Cl1 O14 1.443(4) . ?
Cl1 O11 1.443(4) . ?
Cl2 O21 1.303(9) . ?
Cl2 O22 1.335(7) . ?
Cl2 O23 1.416(7) . ?
Cl2 O24 1.425(5) . ?
C1 Cl11 1.742(6) . ?
C1 Cl13 1.746(6) . ?
C1 Cl12 1.748(7) . ?
C2 Cl22 1.714(5) . ?
C2 Cl21 1.733(6) . ?
C2 Cl23 1.770(6) . ?
