#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:07:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178491 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060257.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_4060257
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om034268l
_journal_year                    2004
_chemical_formula_sum            'C46 H90 B20 Li N2 O6 P2 Sm'
_chemical_formula_weight         1202.63
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.994(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.160(3)
_cell_length_b                   18.178(3)
_cell_length_c                   21.215(4)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     6824(2)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36456
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         12030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1459P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2304
_reflns_number_gt                7921
_reflns_number_total             12030
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060257
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
Sm1 Sm 0.87533(2) 0.209192(18) 0.491763(17) 0.04806(17) Uani 1 1 d . . .
P2 P 0.78095(13) 0.09096(11) 0.60892(10) 0.0587(5) Uani 1 1 d . . .
P1 P 0.92647(13) 0.31093(11) 0.34614(9) 0.0581(5) Uani 1 1 d . . .
Li1 Li 0.3611(11) 0.3319(9) 0.5249(10) 0.098(5) Uani 1 1 d . . .
N1 N 0.9553(4) 0.3951(4) 0.3310(3) 0.0689(18) Uani 1 1 d . . .
N2 N 0.8207(6) 0.0437(4) 0.6765(3) 0.088(3) Uani 1 1 d . . .
B3 B 0.7740(5) 0.3674(5) 0.3820(4) 0.063(2) Uani 1 1 d . . .
H3 H 0.8019 0.4073 0.4186 0.076 Uiso 1 1 calc R . .
B4 B 0.7635(6) 0.3832(6) 0.2977(4) 0.071(3) Uani 1 1 d . . .
H4 H 0.7845 0.4334 0.2788 0.085 Uiso 1 1 calc R . .
B5 B 0.7677(7) 0.2958(6) 0.2613(5) 0.082(3) Uani 1 1 d . . .
H5 H 0.7905 0.2892 0.2178 0.099 Uiso 1 1 calc R . .
B6 B 0.7838(6) 0.2290(5) 0.3240(6) 0.076(3) Uani 1 1 d . . .
H6 H 0.8181 0.1794 0.3225 0.091 Uiso 1 1 calc R . .
B7 B 0.6966(6) 0.3149(6) 0.3912(5) 0.076(3) Uani 1 1 d . . .
H7 H 0.6723 0.3207 0.4340 0.091 Uiso 1 1 calc R . .
B8 B 0.6830(6) 0.3829(6) 0.3312(5) 0.077(3) Uani 1 1 d . . .
H8 H 0.6507 0.4334 0.3346 0.093 Uiso 1 1 calc R . .
B9 B 0.6796(7) 0.3391(7) 0.2568(5) 0.038(3) Uani 0.54 1 d P . .
H9 H 0.6449 0.3607 0.2113 0.045 Uiso 0.54 1 calc PR . .
B10 B 0.6945(7) 0.2411(8) 0.2738(6) 0.091(3) Uiso 1 1 d . . .
H10 H 0.6699 0.1978 0.2392 0.110 Uiso 1 1 calc R . .
B11 B 0.7028(6) 0.2305(6) 0.3564(6) 0.082(3) Uani 1 1 d . . .
H11 H 0.6823 0.1807 0.3763 0.099 Uiso 1 1 calc R . .
B12 B 0.6385(7) 0.2969(6) 0.3144(6) 0.087(3) Uani 1 1 d . . .
H12 H 0.5768 0.2908 0.3056 0.104 Uiso 1 1 calc R . .
B23 B 0.8661(6) 0.2361(6) 0.6752(5) 0.072(3) Uani 1 1 d . . .
H23 H 0.9199 0.2090 0.6970 0.087 Uiso 1 1 calc R . .
B24 B 0.7807(7) 0.2228(6) 0.7032(5) 0.079(3) Uani 1 1 d . . .
H24 H 0.7797 0.1869 0.7447 0.094 Uiso 1 1 calc R . .
B25 B 0.7043(7) 0.2284(6) 0.6364(5) 0.075(3) Uani 1 1 d . . .
H25 H 0.6523 0.1964 0.6338 0.091 Uiso 1 1 calc R . .
B26 B 0.7439(7) 0.2438(5) 0.5694(5) 0.072(3) Uani 1 1 d . . .
H26 H 0.7185 0.2206 0.5216 0.087 Uiso 1 1 calc R . .
B27 B 0.8623(8) 0.3251(6) 0.6436(6) 0.089(4) Uani 1 1 d . . .
H27 H 0.9143 0.3570 0.6460 0.107 Uiso 1 1 calc R . .
B28 B 0.8260(8) 0.3090(6) 0.7125(6) 0.089(4) Uani 1 1 d . . .
H28 H 0.8542 0.3300 0.7605 0.107 Uiso 1 1 calc R . .
B29 B 0.7256(8) 0.3050(6) 0.6882(6) 0.088(4) Uani 1 1 d . . .
H29 H 0.6885 0.3236 0.7195 0.106 Uiso 1 1 calc R . .
B30 B 0.7001(8) 0.3162(6) 0.6022(6) 0.090(4) Uani 1 1 d . . .
H30 H 0.6465 0.3411 0.5767 0.108 Uiso 1 1 calc R . .
B31 B 0.7879(7) 0.3297(6) 0.5776(5) 0.082(3) Uani 1 1 d . . .
H31 H 0.7909 0.3652 0.5362 0.098 Uiso 1 1 calc R . .
B32 B 0.7772(8) 0.3678(6) 0.6519(6) 0.094(4) Uani 1 1 d . . .
H32 H 0.7729 0.4273 0.6598 0.113 Uiso 1 1 calc R . .
O1 O 0.3643(6) 0.2180(4) 0.5409(6) 0.152(4) Uani 1 1 d . . .
O2 O 0.4508(9) 0.3013(7) 0.4789(10) 0.237(8) Uani 1 1 d . . .
O3 O 0.4348(9) 0.3546(7) 0.6221(7) 0.249(8) Uani 1 1 d . . .
O4 O 0.2752(5) 0.3517(6) 0.5836(5) 0.158(4) Uani 1 1 d . . .
O5 O 0.2706(9) 0.3208(8) 0.4406(5) 0.209(6) Uani 1 1 d . . .
O6 O 0.3622(7) 0.4449(5) 0.4960(5) 0.177(5) Uani 1 1 d . . .
C1 C 0.8206(5) 0.3158(4) 0.3379(3) 0.062(2) Uani 1 1 d . . .
C2 C 0.7839(5) 0.2751(4) 0.3951(4) 0.063(2) Uani 1 1 d . . .
C3 C 0.9972(6) 0.4033(6) 0.2800(5) 0.093(3) Uani 1 1 d . . .
H3A H 1.0190 0.4529 0.2835 0.111 Uiso 1 1 calc R . .
C4 C 1.0624(7) 0.3482(9) 0.2882(6) 0.140(5) Uani 1 1 d . . .
H4A H 1.0945 0.3535 0.3305 0.210 Uiso 1 1 calc R . .
H4B H 1.0910 0.3575 0.2561 0.210 Uiso 1 1 calc R . .
H4C H 1.0424 0.2991 0.2830 0.210 Uiso 1 1 calc R . .
C5 C 0.9462(8) 0.3965(9) 0.2148(5) 0.147(6) Uani 1 1 d . . .
H5A H 0.9751 0.4010 0.1823 0.221 Uiso 1 1 calc R . .
H5B H 0.9087 0.4346 0.2091 0.221 Uiso 1 1 calc R . .
H5C H 0.9217 0.3493 0.2110 0.221 Uiso 1 1 calc R . .
C6 C 0.9584(6) 0.4597(5) 0.3737(5) 0.088(3) Uani 1 1 d . . .
H6A H 0.9248 0.4487 0.4027 0.106 Uiso 1 1 calc R . .
C7 C 0.9266(7) 0.5311(5) 0.3360(7) 0.128(4) Uani 1 1 d . . .
H7A H 0.8774 0.5213 0.3094 0.192 Uiso 1 1 calc R . .
H7B H 0.9599 0.5463 0.3091 0.192 Uiso 1 1 calc R . .
H7C H 0.9230 0.5695 0.3662 0.192 Uiso 1 1 calc R . .
C8 C 1.0350(7) 0.4733(6) 0.4164(5) 0.112(4) Uani 1 1 d . . .
H8A H 1.0532 0.4290 0.4393 0.167 Uiso 1 1 calc R . .
H8B H 1.0316 0.5115 0.4468 0.167 Uiso 1 1 calc R . .
H8C H 1.0694 0.4880 0.3903 0.167 Uiso 1 1 calc R . .
C11 C 0.9581(5) 0.2956(3) 0.4328(4) 0.0534(18) Uani 1 1 d . . .
C12 C 0.9480(4) 0.3349(4) 0.4876(3) 0.0571(18) Uani 1 1 d . . .
H12A H 0.9248 0.3837 0.4862 0.069 Uiso 1 1 calc R . .
C13 C 0.9906(5) 0.3020(4) 0.5432(4) 0.065(2) Uani 1 1 d . . .
H13A H 0.9996 0.3232 0.5867 0.077 Uiso 1 1 calc R . .
C14 C 1.0860(6) 0.1946(5) 0.5599(5) 0.084(3) Uani 1 1 d . . .
H14A H 1.0977 0.1968 0.6049 0.101 Uiso 1 1 calc R . .
C15 C 1.1210(6) 0.1453(6) 0.5293(7) 0.101(4) Uani 1 1 d . . .
H15A H 1.1581 0.1145 0.5529 0.121 Uiso 1 1 calc R . .
C16 C 1.1011(5) 0.1405(5) 0.4607(6) 0.087(3) Uani 1 1 d . . .
H16A H 1.1254 0.1061 0.4401 0.105 Uiso 1 1 calc R . .
C17 C 1.0486(5) 0.1837(5) 0.4251(5) 0.073(2) Uani 1 1 d . . .
H17A H 1.0355 0.1787 0.3803 0.088 Uiso 1 1 calc R . .
C18 C 1.0130(4) 0.2377(4) 0.4571(4) 0.0601(19) Uani 1 1 d . . .
C19 C 1.0324(4) 0.2421(4) 0.5245(4) 0.0601(19) Uani 1 1 d . . .
C21 C 0.7871(5) 0.1919(4) 0.6307(4) 0.0593(19) Uani 1 1 d . . .
C22 C 0.8372(5) 0.2517(4) 0.5937(4) 0.062(2) Uani 1 1 d . . .
C23 C 0.9028(7) 0.0451(6) 0.7095(4) 0.102(4) Uani 1 1 d . . .
H23A H 0.9269 0.0852 0.6907 0.123 Uiso 1 1 calc R . .
C24 C 0.9132(9) 0.0604(8) 0.7832(5) 0.155(7) Uani 1 1 d . . .
H24A H 0.8873 0.1050 0.7893 0.233 Uiso 1 1 calc R . .
H24B H 0.9660 0.0655 0.8027 0.233 Uiso 1 1 calc R . .
H24C H 0.8927 0.0202 0.8031 0.233 Uiso 1 1 calc R . .
C25 C 0.9413(8) -0.0266(7) 0.6983(6) 0.130(5) Uani 1 1 d . . .
H25A H 0.9354 -0.0345 0.6527 0.196 Uiso 1 1 calc R . .
H25B H 0.9187 -0.0667 0.7166 0.196 Uiso 1 1 calc R . .
H25C H 0.9941 -0.0239 0.7186 0.196 Uiso 1 1 calc R . .
C26 C 0.7677(8) -0.0118(6) 0.6949(6) 0.120(5) Uani 1 1 d . . .
H26A H 0.7967 -0.0371 0.7333 0.144 Uiso 1 1 calc R . .
C27 C 0.7435(8) -0.0705(6) 0.6446(6) 0.135(5) Uani 1 1 d . . .
H27A H 0.7872 -0.0907 0.6325 0.202 Uiso 1 1 calc R . .
H27B H 0.7104 -0.0495 0.6072 0.202 Uiso 1 1 calc R . .
H27C H 0.7174 -0.1088 0.6619 0.202 Uiso 1 1 calc R . .
C28 C 0.7012(8) 0.0268(6) 0.7166(6) 0.136(5) Uani 1 1 d . . .
H28A H 0.7208 0.0636 0.7484 0.203 Uiso 1 1 calc R . .
H28B H 0.6731 -0.0089 0.7349 0.203 Uiso 1 1 calc R . .
H28C H 0.6686 0.0496 0.6799 0.203 Uiso 1 1 calc R . .
C31 C 0.8428(4) 0.0851(3) 0.5547(3) 0.0502(17) Uani 1 1 d . . .
C32 C 0.9225(5) 0.0896(4) 0.5632(4) 0.0596(19) Uani 1 1 d . . .
H32A H 0.9579 0.0910 0.6055 0.072 Uiso 1 1 calc R . .
C33 C 0.9435(5) 0.0759(4) 0.5060(5) 0.072(2) Uani 1 1 d . . .
H33A H 0.9954 0.0665 0.5021 0.086 Uiso 1 1 calc R . .
C34 C 0.8665(9) 0.0374(5) 0.3942(5) 0.103(4) Uani 1 1 d . . .
H34A H 0.9068 0.0355 0.3738 0.123 Uiso 1 1 calc R . .
C35 C 0.7968(11) 0.0197(6) 0.3612(5) 0.118(5) Uani 1 1 d . . .
H35A H 0.7900 0.0051 0.3182 0.142 Uiso 1 1 calc R . .
C36 C 0.7357(9) 0.0224(6) 0.3884(6) 0.114(4) Uani 1 1 d . . .
H36A H 0.6879 0.0098 0.3645 0.137 Uiso 1 1 calc R . .
C37 C 0.7463(6) 0.0448(4) 0.4538(4) 0.079(3) Uani 1 1 d . . .
H37A H 0.7048 0.0466 0.4727 0.095 Uiso 1 1 calc R . .
C38 C 0.8146(5) 0.0636(4) 0.4892(3) 0.0555(18) Uani 1 1 d . . .
C39 C 0.8790(3) 0.0585(3) 0.4591(3) 0.065(2) Uani 1 1 d . . .
C41 C 0.3086(3) 0.1752(3) 0.5617(3) 0.166(6) Uiso 1 1 d R . .
H41A H 0.3243 0.1247 0.5657 0.249 Uiso 1 1 calc R . .
H41B H 0.2614 0.1791 0.5306 0.249 Uiso 1 1 calc R . .
H41C H 0.3025 0.1930 0.6028 0.249 Uiso 1 1 calc R . .
C42 C 0.4147(3) 0.1750(3) 0.5299(3) 0.278(13) Uiso 1 1 d R . .
H42A H 0.3929 0.1307 0.5079 0.333 Uiso 1 1 calc R . .
H42B H 0.4505 0.1617 0.5695 0.333 Uiso 1 1 calc R . .
C43 C 0.4577(3) 0.2307(3) 0.4790(3) 0.318(17) Uiso 1 1 d R . .
H43A H 0.5114 0.2199 0.4898 0.381 Uiso 1 1 calc R . .
H43B H 0.4385 0.2141 0.4349 0.381 Uiso 1 1 calc R . .
C44 C 0.4909(3) 0.3277(3) 0.4389(3) 0.198(8) Uiso 1 1 d R . .
H44A H 0.5280 0.2921 0.4335 0.296 Uiso 1 1 calc R . .
H44B H 0.5158 0.3722 0.4566 0.296 Uiso 1 1 calc R . .
H44C H 0.4580 0.3381 0.3977 0.296 Uiso 1 1 calc R . .
C45 C 0.5055(3) 0.3223(3) 0.6544(3) 0.300(14) Uiso 1 1 d R . .
H45A H 0.5217 0.3436 0.6967 0.450 Uiso 1 1 calc R . .
H45B H 0.5428 0.3317 0.6297 0.450 Uiso 1 1 calc R . .
H45C H 0.4992 0.2702 0.6583 0.450 Uiso 1 1 calc R . .
C46 C 0.3921(3) 0.3552(3) 0.6767(3) 0.035(7) Uiso 0.17 1 d PR . .
H46A H 0.3984 0.3077 0.6980 0.042 Uiso 0.17 1 calc PR . .
H46B H 0.4148 0.3919 0.7083 0.042 Uiso 0.17 1 calc PR . .
C47 C 0.3133(3) 0.3703(3) 0.6561(3) 0.213(8) Uiso 1 1 d R . .
H47A H 0.3055 0.4222 0.6631 0.255 Uiso 1 1 calc R . .
H47B H 0.2871 0.3430 0.6837 0.255 Uiso 1 1 calc R . .
C48 C 0.1989(3) 0.3640(3) 0.5531(3) 0.262(11) Uiso 1 1 d R . .
H48A H 0.1701 0.3715 0.5853 0.393 Uiso 1 1 calc R . .
H48B H 0.1795 0.3221 0.5271 0.393 Uiso 1 1 calc R . .
H48C H 0.1952 0.4069 0.5261 0.393 Uiso 1 1 calc R . .
C49 C 0.2566(3) 0.2715(3) 0.3939(3) 0.276(14) Uiso 1 1 d R . .
H49A H 0.2116 0.2850 0.3628 0.414 Uiso 1 1 calc R . .
H49B H 0.2497 0.2242 0.4117 0.414 Uiso 1 1 calc R . .
H49C H 0.2984 0.2694 0.3731 0.414 Uiso 1 1 calc R . .
C50 C 0.2809(3) 0.3995(3) 0.4011(3) 0.339(16) Uiso 1 1 d R . .
H50A H 0.3125 0.3902 0.3707 0.407 Uiso 1 1 calc R . .
H50B H 0.2318 0.4156 0.3766 0.407 Uiso 1 1 calc R . .
C51 C 0.3146(3) 0.4577(3) 0.4453(3) 0.029(10) Uiso 0.12 1 d PR . .
H51A H 0.3377 0.4920 0.4205 0.035 Uiso 0.12 1 calc PR . .
H51B H 0.2733 0.4837 0.4576 0.035 Uiso 0.12 1 calc PR . .
C52 C 0.4064(3) 0.5006(3) 0.5491(3) 0.44(2) Uiso 1 1 d R . .
H52A H 0.4032 0.5494 0.5314 0.660 Uiso 1 1 calc R . .
H52B H 0.4585 0.4861 0.5619 0.660 Uiso 1 1 calc R . .
H52C H 0.3842 0.4999 0.5861 0.660 Uiso 1 1 calc R . .
