#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:18:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178621 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/32/4073218.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_4073218
loop_
_publ_author_name
'Evans, William J.'
'Montalvo, Elizabeth'
'Foster, Samuel E.'
'Harada, Kimberly A.'
'Ziller, Joseph W.'
_publ_section_title
;
 Reactivity of (C5Me5)2Sm(THF)2with Nitriles:  C−C Bond
 Cleavage To Form Cyanide Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2904
_journal_paper_doi               10.1021/om070176a
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '[(C5Me5)2Sm(NCCMe3)(-CN)]3'
_chemical_formula_sum            'C99 H141 N6 Sm3'
_chemical_formula_weight         1866.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   20.3157(8)
_cell_length_b                   20.3157(8)
_cell_length_c                   14.2464(9)
_cell_measurement_temperature    163(2)
_cell_volume                     5092.1(4)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27257
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  0.7211
_exptl_absorpt_correction_T_min  0.5561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1926
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.466
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.242
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3030
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1072P)²+17.7057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                2241
_reflns_number_total             3030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070176a-file001.cif
_cod_data_source_block           kh1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_H-M      P6(3)/m
_cod_database_code               4073218
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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 0.45978(3) 0.24885(4) 0.2500 0.0355(3) Uani 1 2 d S . .
N1 N 0.4326(6) 0.3589(6) 0.2500 0.048(3) Uani 1 2 d S . .
N2 N 0.6481(7) 0.4331(7) 0.2500 0.052(3) Uani 1 2 d S . .
C1 C 0.4375(5) 0.2722(5) 0.4334(6) 0.046(2) Uani 1 1 d . . .
C2 C 0.4731(5) 0.2264(5) 0.4359(7) 0.045(2) Uani 1 1 d . . .
C3 C 0.4187(6) 0.1524(5) 0.4011(7) 0.052(2) Uani 1 1 d . . .
C4 C 0.3512(5) 0.1548(6) 0.3812(7) 0.059(3) Uani 1 1 d . . .
C5 C 0.3621(5) 0.2261(6) 0.3990(7) 0.054(3) Uani 1 1 d . . .
C6 C 0.4732(6) 0.3528(6) 0.4691(8) 0.062(3) Uani 1 1 d . . .
H6A H 0.5257 0.3702 0.4885 0.093 Uiso 1 1 calc R . .
H6B H 0.4442 0.3547 0.5229 0.093 Uiso 1 1 calc R . .
H6C H 0.4731 0.3858 0.4191 0.093 Uiso 1 1 calc R . .
C7 C 0.5502(5) 0.2497(6) 0.4744(7) 0.052(2) Uani 1 1 d . . .
H7A H 0.5753 0.3033 0.4930 0.078 Uiso 1 1 calc R . .
H7B H 0.5806 0.2428 0.4262 0.078 Uiso 1 1 calc R . .
H7C H 0.5451 0.2183 0.5292 0.078 Uiso 1 1 calc R . .
C8 C 0.4312(7) 0.0856(6) 0.3978(8) 0.068(3) Uani 1 1 d . . .
H8A H 0.4837 0.1019 0.4161 0.103 Uiso 1 1 calc R . .
H8B H 0.4221 0.0650 0.3339 0.103 Uiso 1 1 calc R . .
H8C H 0.3961 0.0463 0.4412 0.103 Uiso 1 1 calc R . .
C9 C 0.2737(7) 0.0821(8) 0.3632(9) 0.102(5) Uani 1 1 d . . .
H9A H 0.2817 0.0390 0.3521 0.153 Uiso 1 1 calc R . .
H9B H 0.2495 0.0898 0.3080 0.153 Uiso 1 1 calc R . .
H9C H 0.2408 0.0715 0.4180 0.153 Uiso 1 1 calc R . .
C10 C 0.3026(6) 0.2482(8) 0.3952(9) 0.080(4) Uani 1 1 d . . .
H10A H 0.3251 0.3021 0.4111 0.121 Uiso 1 1 calc R . .
H10B H 0.2622 0.2175 0.4401 0.121 Uiso 1 1 calc R . .
H10C H 0.2812 0.2395 0.3317 0.121 Uiso 1 1 calc R . .
C11 C 0.4204(7) 0.4095(8) 0.2500 0.046(3) Uani 1 2 d S A .
C12 C 0.4061(7) 0.4729(7) 0.2500 0.054(4) Uani 1 2 d SD . .
C13 C 0.3217(9) 0.441(4) 0.2500 0.19(3) Uiso 0.50 2 d SPD A 1
H13A H 0.3107 0.4829 0.2500 0.289 Uiso 0.50 2 calc SPR A 1
H13B H 0.2996 0.4098 0.3062 0.289 Uiso 0.25 1 calc PR A 1
H13C H 0.2996 0.4098 0.1938 0.289 Uiso 0.25 1 calc PR A 1
C14 C 0.4491(15) 0.5249(15) 0.3298(15) 0.100(9) Uiso 0.50 1 d PD A 1
H14A H 0.4399 0.5679 0.3306 0.150 Uiso 0.50 1 calc PR A 1
H14B H 0.5036 0.5438 0.3217 0.150 Uiso 0.50 1 calc PR A 1
H14C H 0.4320 0.4971 0.3892 0.150 Uiso 0.50 1 calc PR A 1
C15 C 0.4812(18) 0.545(2) 0.2500 0.15(2) Uiso 0.50 2 d SPD A 2
H15A H 0.4727 0.5888 0.2500 0.232 Uiso 0.50 2 calc SPR A 2
H15B H 0.5100 0.5473 0.1938 0.232 Uiso 0.25 1 calc PR A 2
H15C H 0.5100 0.5473 0.3062 0.232 Uiso 0.25 1 calc PR A 2
C16 C 0.3712(16) 0.4780(16) 0.3405(11) 0.094(8) Uiso 0.50 1 d PD A 2
H16A H 0.3622 0.5210 0.3379 0.141 Uiso 0.50 1 calc PR A 2
H16B H 0.4058 0.4853 0.3926 0.141 Uiso 0.50 1 calc PR A 2
H16C H 0.3228 0.4309 0.3504 0.141 Uiso 0.50 1 calc PR A 2
C17 C 0.5880(7) 0.3777(6) 0.2500 0.034(3) Uani 1 2 d S . .
C18 C 0.1366(9) -0.1281(9) 0.2985(11) 0.109(5) Uiso 1 1 d . . .
C19 C 0.1915(11) -0.1373(10) 0.3441(15) 0.131(6) Uiso 1 1 d . . .
H19 H 0.1915 -0.1407 0.4106 0.157 Uiso 1 1 calc R . .
C20 C 0.2447(10) -0.1414(10) 0.2935(14) 0.134(6) Uiso 1 1 d . . .
H20 H 0.2841 -0.1444 0.3255 0.160 Uiso 1 1 calc R . .
C21 C 0.100(2) -0.110(2) 0.354(4) 0.152(17) Uiso 0.50 1 d P . .
H21A H 0.0620 -0.1039 0.3192 0.228 Uiso 0.50 1 calc PR . .
H21B H 0.1348 -0.0626 0.3860 0.228 Uiso 0.50 1 calc PR . .
H21C H 0.0742 -0.1507 0.4010 0.228 Uiso 0.50 1 calc PR . .
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'
Sm Sm -0.1638 3.4418 '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
Cnt Sm1 N1 93.9 . .
Cnt Sm1 N2 99.8 . 2_655
Cnt Sm1 C17 112.6 . .
Cnt Sm1 Cnt 134.2 . 10_556
N1 Sm1 N2 144.1(4) . 2_655
N1 Sm1 C17 70.5(3) . .
N2 Sm1 C17 73.6(3) 2_655 .
N1 Sm1 C2 103.3(2) . 10_556
N2 Sm1 C2 77.8(2) 2_655 10_556
C17 Sm1 C2 92.02(19) . 10_556
N1 Sm1 C2 103.3(2) . .
N2 Sm1 C2 77.8(2) 2_655 .
C17 Sm1 C2 92.02(19) . .
C2 Sm1 C2 153.0(4) 10_556 .
N1 Sm1 C1 73.8(2) . .
N2 Sm1 C1 106.3(2) 2_655 .
C17 Sm1 C1 89.7(2) . .
C2 Sm1 C1 175.9(3) 10_556 .
C2 Sm1 C1 30.5(3) . .
N1 Sm1 C1 73.8(2) . 10_556
N2 Sm1 C1 106.3(2) 2_655 10_556
C17 Sm1 C1 89.7(2) . 10_556
C2 Sm1 C1 30.5(3) 10_556 10_556
C2 Sm1 C1 175.9(3) . 10_556
C1 Sm1 C1 145.8(4) . 10_556
N1 Sm1 C3 120.1(2) . 10_556
N2 Sm1 C3 78.9(3) 2_655 10_556
C17 Sm1 C3 120.7(2) . 10_556
C2 Sm1 C3 30.5(3) 10_556 10_556
C2 Sm1 C3 131.6(3) . 10_556
C1 Sm1 C3 148.9(3) . 10_556
C1 Sm1 C3 50.0(3) 10_556 10_556
N1 Sm1 C3 120.1(2) . .
N2 Sm1 C3 78.9(3) 2_655 .
C17 Sm1 C3 120.7(2) . .
C2 Sm1 C3 131.6(3) 10_556 .
C2 Sm1 C3 30.5(3) . .
C1 Sm1 C3 50.0(3) . .
C1 Sm1 C3 148.9(3) 10_556 .
C3 Sm1 C3 103.3(4) 10_556 .
N1 Sm1 C5 72.4(3) . 10_556
N2 Sm1 C5 125.5(2) 2_655 10_556
C17 Sm1 C5 115.9(3) . 10_556
C2 Sm1 C5 49.6(3) 10_556 10_556
C2 Sm1 C5 146.8(3) . 10_556
C1 Sm1 C5 126.3(3) . 10_556
C1 Sm1 C5 29.9(3) 10_556 10_556
C3 Sm1 C5 49.1(3) 10_556 10_556
C3 Sm1 C5 122.9(3) . 10_556
N1 Sm1 C5 72.4(3) . .
N2 Sm1 C5 125.5(2) 2_655 .
C17 Sm1 C5 115.9(3) . .
C2 Sm1 C5 146.8(3) 10_556 .
C2 Sm1 C5 49.6(3) . .
C1 Sm1 C5 29.9(3) . .
C1 Sm1 C5 126.3(3) 10_556 .
C3 Sm1 C5 122.9(3) 10_556 .
C3 Sm1 C5 49.1(3) . .
C5 Sm1 C5 99.5(4) 10_556 .
N1 Sm1 C4 99.0(3) . .
N2 Sm1 C4 107.4(3) 2_655 .
C17 Sm1 C4 137.5(2) . .
C2 Sm1 C4 130.3(3) 10_556 .
C2 Sm1 C4 49.1(3) . .
C1 Sm1 C4 48.4(3) . .
C1 Sm1 C4 128.0(3) 10_556 .
C3 Sm1 C4 100.5(3) 10_556 .
C3 Sm1 C4 29.8(3) . .
C5 Sm1 C4 98.3(3) 10_556 .
C5 Sm1 C4 28.6(3) . .
C11 N1 Sm1 179.7(10) . .
C17 N2 Sm1 170.7(9) . 3_665
C5 C1 C2 107.8(8) . .
C5 C1 C6 127.3(9) . .
C2 C1 C6 124.7(8) . .
C5 C1 Sm1 76.9(5) . .
C2 C1 Sm1 74.3(5) . .
C6 C1 Sm1 118.6(6) . .
C1 C2 C3 107.2(8) . .
C1 C2 C7 126.2(8) . .
C3 C2 C7 126.4(9) . .
C1 C2 Sm1 75.2(5) . .
C3 C2 Sm1 75.6(5) . .
C7 C2 Sm1 118.7(6) . .
C4 C3 C2 106.5(9) . .
C4 C3 C8 128.7(9) . .
C2 C3 C8 124.5(9) . .
C4 C3 Sm1 77.0(5) . .
C2 C3 Sm1 73.9(5) . .
C8 C3 Sm1 119.5(7) . .
C5 C4 C3 110.4(9) . .
C5 C4 C9 125.8(11) . .
C3 C4 C9 122.6(11) . .
C5 C4 Sm1 75.3(5) . .
C3 C4 Sm1 73.3(5) . .
C9 C4 Sm1 128.3(7) . .
C4 C5 C1 108.1(9) . .
C4 C5 C10 125.7(10) . .
C1 C5 C10 125.7(10) . .
C4 C5 Sm1 76.1(6) . .
C1 C5 Sm1 73.2(5) . .
C10 C5 Sm1 122.9(7) . .
N1 C11 C12 179.5(14) . .
C11 C12 C16 111.8(12) . 10_556
C11 C12 C16 111.8(12) . .
C16 C12 C16 119(2) 10_556 .
C11 C12 C13 108(3) . .
C16 C12 C13 63.4(14) 10_556 .
C16 C12 C13 63.4(14) . .
C11 C12 C15 108(3) . .
C16 C12 C15 102.5(17) 10_556 .
C16 C12 C15 102.5(17) . .
C13 C12 C15 144(4) . .
C11 C12 C14 108.6(14) . 10_556
C16 C12 C14 55.2(15) 10_556 10_556
C16 C12 C14 137.1(19) . 10_556
C13 C12 C14 116(2) . 10_556
C15 C12 C14 50.2(13) . 10_556
C11 C12 C14 108.6(14) . .
C16 C12 C14 137.1(19) 10_556 .
C16 C12 C14 55.2(15) . .
C13 C12 C14 116(2) . .
C15 C12 C14 50.2(13) . .
C14 C12 C14 99(3) 10_556 .
N2 C17 Sm1 175.7(10) . .
C21 C18 C19 112(3) . .
C21 C18 C18 129(2) . 10_556
C19 C18 C18 118.0(11) . 10_556
C20 C19 C18 119(2) . .
C20 C20 C19 122.7(13) 10_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 Cnt 2.477 .
Sm1 N1 2.558(12) .
Sm1 N2 2.589(13) 2_655
Sm1 C17 2.612(12) .
Sm1 C2 2.723(9) 10_556
Sm1 C2 2.723(9) .
Sm1 C1 2.734(9) .
Sm1 C1 2.734(9) 10_556
Sm1 C3 2.745(9) 10_556
Sm1 C3 2.745(9) .
Sm1 C5 2.782(9) 10_556
Sm1 C5 2.782(9) .
Sm1 C4 2.792(9) .
N1 C11 1.171(16) .
N2 C17 1.175(16) .
N2 Sm1 2.589(13) 3_665
C1 C5 1.424(13) .
C1 C2 1.437(14) .
C1 C6 1.508(14) .
C2 C3 1.437(13) .
C2 C7 1.496(13) .
C3 C4 1.423(14) .
C3 C8 1.502(14) .
C4 C5 1.376(15) .
C4 C9 1.550(15) .
C5 C10 1.487(14) .
C11 C12 1.455(18) .
C12 C16 1.4999(10) 10_556
C12 C16 1.4999(10) .
C12 C13 1.5000(10) .
C12 C15 1.5001(10) .
C12 C14 1.5001(10) 10_556
C12 C14 1.5001(10) .
C18 C21 1.26(4) .
C18 C19 1.38(2) .
C18 C18 1.38(3) 10_556
C19 C20 1.33(2) .
C20 C20 1.24(4) 10_556
