#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:32:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180144 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/41/7104111.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_7104111
loop_
_publ_author_name
'Jones, Cameron'
'Stasch, Andreas'
'Woodul, William D'
_publ_section_title
;
 Gallyl lanthanide complexes containing unsupported Ln-Ga (Ln = Sm, Eu,
 Yb or Tm) bonds.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              113
_journal_page_last               115
_journal_paper_doi               10.1039/b817933f
_journal_volume                  34
_journal_year                    2008
_chemical_formula_sum            'C64 H104 Ga2 N8 Sm'
_chemical_formula_weight         1275.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 131.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.344(6)
_cell_length_b                   13.855(3)
_cell_length_c                   21.633(4)
_cell_measurement_temperature    123(2)
_cell_volume                     6589(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 CCd'
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41996
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.782
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         9610
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+15.1112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                8436
_reflns_number_total             9610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817933f.txt
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7104111
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
Sm1 Sm 0.0000 0.0000 0.0000 0.02206(5) Uani 1 2 d S . .
Ga1 Ga 0.111816(9) 0.159860(16) 0.093408(14) 0.02187(6) Uani 1 1 d . . .
N1 N 0.14848(8) 0.25395(13) 0.18047(11) 0.0256(3) Uani 1 1 d . . .
C1 C 0.18876(12) 0.31387(19) 0.18549(16) 0.0386(6) Uani 1 1 d . . .
H1 H 0.2108 0.3633 0.2259 0.046 Uiso 1 1 calc R . .
N2 N 0.16114(9) 0.22177(14) 0.07531(12) 0.0278(4) Uani 1 1 d . . .
C2 C 0.19473(13) 0.2978(2) 0.12984(17) 0.0413(6) Uani 1 1 d . . .
H2 H 0.2205 0.3364 0.1279 0.050 Uiso 1 1 calc R . .
N3 N 0.00390(14) -0.0014(2) 0.12825(18) 0.0553(8) Uani 1 1 d . . .
C3 C 0.14434(11) 0.26141(18) 0.24224(15) 0.0323(5) Uani 1 1 d . . .
N4 N 0.07439(12) -0.1462(2) 0.10754(16) 0.0534(6) Uani 1 1 d . . .
C4 C 0.09589(13) 0.3118(2) 0.22542(19) 0.0462(7) Uani 1 1 d . . .
C5 C 0.09179(17) 0.3145(3) 0.2865(2) 0.0628(10) Uani 1 1 d . . .
H5 H 0.0592 0.3486 0.2761 0.075 Uiso 1 1 calc R . .
C6 C 0.1333(2) 0.2693(3) 0.3599(2) 0.0734(13) Uani 1 1 d . . .
H6 H 0.1295 0.2720 0.4001 0.088 Uiso 1 1 calc R . .
C7 C 0.18082(18) 0.2199(3) 0.3767(2) 0.0594(9) Uani 1 1 d . . .
H7 H 0.2094 0.1883 0.4284 0.071 Uiso 1 1 calc R . .
C8 C 0.18798(14) 0.2150(2) 0.31883(16) 0.0412(6) Uani 1 1 d . . .
C9 C 0.04986(12) 0.3618(3) 0.1437(2) 0.0539(8) Uani 1 1 d . . .
H9 H 0.0474 0.3242 0.1021 0.065 Uiso 1 1 calc R . .
C10 C -0.01441(16) 0.3658(3) 0.1128(3) 0.0822(14) Uani 1 1 d . . .
H10A H -0.0294 0.3000 0.1060 0.123 Uiso 1 1 calc R . .
H10B H -0.0414 0.3994 0.0596 0.123 Uiso 1 1 calc R . .
H10C H -0.0137 0.4006 0.1529 0.123 Uiso 1 1 calc R . .
C11 C 0.06979(18) 0.4624(4) 0.1447(3) 0.0800(12) Uani 1 1 d . . .
H11A H 0.0752 0.5006 0.1873 0.120 Uiso 1 1 calc R . .
H11B H 0.0388 0.4927 0.0908 0.120 Uiso 1 1 calc R . .
H11C H 0.1084 0.4594 0.1568 0.120 Uiso 1 1 calc R . .
C12 C 0.24071(14) 0.1593(2) 0.33759(17) 0.0463(6) Uani 1 1 d . . .
H12 H 0.2477 0.1867 0.3017 0.056 Uiso 1 1 calc R . .
C13 C 0.30099(19) 0.1680(3) 0.4275(2) 0.0793(13) Uani 1 1 d . . .
H13A H 0.3113 0.2363 0.4421 0.119 Uiso 1 1 calc R . .
H13B H 0.3334 0.1356 0.4335 0.119 Uiso 1 1 calc R . .
H13C H 0.2966 0.1376 0.4642 0.119 Uiso 1 1 calc R . .
C14 C 0.22499(17) 0.0528(2) 0.3152(2) 0.0579(8) Uani 1 1 d . . .
H14A H 0.2154 0.0244 0.3470 0.087 Uiso 1 1 calc R . .
H14B H 0.2598 0.0190 0.3282 0.087 Uiso 1 1 calc R . .
H14C H 0.1897 0.0467 0.2561 0.087 Uiso 1 1 calc R . .
C15 C 0.16812(9) 0.20074(15) 0.01772(13) 0.0247(4) Uani 1 1 d . A .
C16 C 0.14445(13) 0.26345(17) -0.04868(16) 0.0353(5) Uani 1 1 d D . .
C17 C 0.15318(12) 0.24123(18) -0.10300(15) 0.0353(5) Uani 1 1 d . A .
H17 H 0.1379 0.2839 -0.1474 0.042 Uiso 1 1 calc R . .
C18 C 0.18320(11) 0.15942(19) -0.09382(14) 0.0342(5) Uani 1 1 d . . .
H18 H 0.1889 0.1457 -0.1313 0.041 Uiso 1 1 calc R A .
C19 C 0.20512(11) 0.0969(2) -0.02968(15) 0.0365(5) Uani 1 1 d . A .
H19 H 0.2252 0.0395 -0.0241 0.044 Uiso 1 1 calc R . .
C20 C 0.19833(10) 0.11635(18) 0.02702(13) 0.0288(4) Uani 1 1 d . . .
C21 C 0.1229(4) 0.3592(5) -0.0493(5) 0.0281(14) Uani 0.419(8) 1 d PD A 1
H21 H 0.1469 0.3822 0.0087 0.034 Uiso 0.419(8) 1 calc PR A 1
C22 C 0.1237(4) 0.4361(5) -0.0991(5) 0.0407(17) Uani 0.419(8) 1 d PD A 1
H22A H 0.1653 0.4441 -0.0772 0.061 Uiso 0.419(8) 1 calc PR A 1
H22B H 0.1092 0.4975 -0.0951 0.061 Uiso 0.419(8) 1 calc PR A 1
H22C H 0.0970 0.4161 -0.1570 0.061 Uiso 0.419(8) 1 calc PR A 1
C23A C 0.0382(2) 0.3516(4) -0.1597(4) 0.0530(16) Uani 0.581(8) 1 d PD A 2
H23A H 0.0124 0.4015 -0.1644 0.079 Uiso 0.581(8) 1 calc PR A 2
H23B H 0.0183 0.2886 -0.1733 0.079 Uiso 0.581(8) 1 calc PR A 2
H23C H 0.0444 0.3660 -0.1980 0.079 Uiso 0.581(8) 1 calc PR A 2
C24 C 0.22447(13) 0.0483(2) 0.09898(17) 0.0415(6) Uani 1 1 d . A .
H24 H 0.1931 0.0415 0.1040 0.050 Uiso 1 1 calc R . .
C25 C 0.28120(14) 0.0910(3) 0.18021(19) 0.0657(11) Uani 1 1 d . . .
H25A H 0.2948 0.0485 0.2259 0.099 Uiso 1 1 calc R A .
H25B H 0.2716 0.1549 0.1885 0.099 Uiso 1 1 calc R . .
H25C H 0.3136 0.0971 0.1784 0.099 Uiso 1 1 calc R . .
C26 C 0.2375(2) -0.0524(3) 0.0862(3) 0.0691(12) Uani 1 1 d . . .
H26A H 0.2723 -0.0500 0.0892 0.104 Uiso 1 1 calc R A .
H26B H 0.2017 -0.0765 0.0319 0.104 Uiso 1 1 calc R . .
H26C H 0.2468 -0.0955 0.1292 0.104 Uiso 1 1 calc R . .
C27 C 0.0247(3) -0.0990(4) 0.1628(3) 0.108(2) Uani 1 1 d . . .
H27A H -0.0090 -0.1446 0.1244 0.130 Uiso 1 1 calc R . .
H27B H 0.0334 -0.1010 0.2155 0.130 Uiso 1 1 calc R . .
C28 C 0.0788(2) -0.1334(4) 0.1782(2) 0.0771(13) Uani 1 1 d . . .
H28A H 0.1123 -0.0875 0.2166 0.093 Uiso 1 1 calc R . .
H28B H 0.0907 -0.1962 0.2072 0.093 Uiso 1 1 calc R . .
C29 C 0.0349(2) 0.0773(3) 0.1824(3) 0.0832(15) Uani 1 1 d . . .
H29A H 0.0358 0.0701 0.2283 0.125 Uiso 1 1 calc R . .
H29B H 0.0139 0.1374 0.1527 0.125 Uiso 1 1 calc R . .
H29C H 0.0766 0.0794 0.2040 0.125 Uiso 1 1 calc R . .
C30 C -0.0583(2) 0.0022(5) 0.0971(3) 0.129(3) Uani 1 1 d . . .
H30A H -0.0572 -0.0070 0.1429 0.194 Uiso 1 1 calc R . .
H30B H -0.0827 -0.0491 0.0562 0.194 Uiso 1 1 calc R . .
H30C H -0.0764 0.0651 0.0712 0.194 Uiso 1 1 calc R . .
C31 C 0.1343(2) -0.1364(4) 0.1326(3) 0.0923(16) Uani 1 1 d . . .
H31A H 0.1609 -0.1886 0.1707 0.139 Uiso 1 1 calc R . .
H31B H 0.1521 -0.0741 0.1601 0.139 Uiso 1 1 calc R . .
H31C H 0.1301 -0.1398 0.0838 0.139 Uiso 1 1 calc R . .
C32 C 0.0524(2) -0.2414(3) 0.0742(3) 0.103(2) Uani 1 1 d . . .
H32A H 0.0827 -0.2892 0.1144 0.155 Uiso 1 1 calc R . .
H32B H 0.0452 -0.2475 0.0233 0.155 Uiso 1 1 calc R . .
H32C H 0.0142 -0.2526 0.0623 0.155 Uiso 1 1 calc R . .
C23 C 0.0574(3) 0.3403(6) -0.0888(6) 0.063(3) Uani 0.419(8) 1 d PD A 1
H23D H 0.0363 0.3052 -0.1407 0.094 Uiso 0.419(8) 1 calc PR A 1
H23E H 0.0368 0.4019 -0.0997 0.094 Uiso 0.419(8) 1 calc PR A 1
H23F H 0.0570 0.3015 -0.0512 0.094 Uiso 0.419(8) 1 calc PR A 1
C22A C 0.1334(3) 0.4451(4) -0.0552(6) 0.0578(19) Uani 0.581(8) 1 d PD A 2
H22D H 0.1399 0.4512 -0.0940 0.087 Uiso 0.581(8) 1 calc PR A 2
H22E H 0.1728 0.4446 0.0014 0.087 Uiso 0.581(8) 1 calc PR A 2
H22F H 0.1092 0.4999 -0.0622 0.087 Uiso 0.581(8) 1 calc PR A 2
C21A C 0.0990(3) 0.3496(4) -0.0723(4) 0.0355(13) Uani 0.581(8) 1 d PD A 2
H21A H 0.0911 0.3468 -0.0339 0.043 Uiso 0.581(8) 1 calc PR A 2
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'
Ga Ga 0.2307 1.6083 '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
_geom_angle_publ_flag
N3 Sm1 N3 180.00(13) . 5 ?
N3 Sm1 N4 110.14(10) . 5 ?
N3 Sm1 N4 69.86(10) 5 5 ?
N3 Sm1 N4 69.86(10) . . ?
N3 Sm1 N4 110.14(10) 5 . ?
N4 Sm1 N4 180.00(8) 5 . ?
N3 Sm1 Ga1 88.44(6) . 5 ?
N3 Sm1 Ga1 91.56(6) 5 5 ?
N4 Sm1 Ga1 93.78(7) 5 5 ?
N4 Sm1 Ga1 86.22(7) . 5 ?
N3 Sm1 Ga1 91.56(6) . . ?
N3 Sm1 Ga1 88.44(6) 5 . ?
N4 Sm1 Ga1 86.22(7) 5 . ?
N4 Sm1 Ga1 93.78(7) . . ?
Ga1 Sm1 Ga1 180.000(9) 5 . ?
N1 Ga1 N2 83.66(8) . . ?
N1 Ga1 Sm1 137.23(5) . . ?
N2 Ga1 Sm1 138.19(5) . . ?
C1 N1 C3 118.73(18) . . ?
C1 N1 Ga1 112.08(14) . . ?
C3 N1 Ga1 128.80(14) . . ?
C2 C1 N1 116.1(2) . . ?
C2 N2 C15 117.82(17) . . ?
C2 N2 Ga1 111.69(14) . . ?
C15 N2 Ga1 130.49(14) . . ?
C1 C2 N2 116.4(2) . . ?
C29 N3 C30 106.1(3) . . ?
C29 N3 C27 118.0(4) . . ?
C30 N3 C27 103.7(4) . . ?
C29 N3 Sm1 114.50(19) . . ?
C30 N3 Sm1 109.5(2) . . ?
C27 N3 Sm1 104.4(2) . . ?
C4 C3 C8 120.6(2) . . ?
C4 C3 N1 119.8(2) . . ?
C8 C3 N1 119.6(2) . . ?
C32 N4 C28 109.6(4) . . ?
C32 N4 C31 107.6(4) . . ?
C28 N4 C31 110.5(3) . . ?
C32 N4 Sm1 114.3(2) . . ?
C28 N4 Sm1 105.5(2) . . ?
C31 N4 Sm1 109.3(2) . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 C9 120.1(2) . . ?
C5 C4 C9 121.6(3) . . ?
C6 C5 C4 121.3(3) . . ?
C5 C6 C7 120.6(3) . . ?
C6 C7 C8 121.1(4) . . ?
C7 C8 C3 118.1(3) . . ?
C7 C8 C12 120.9(3) . . ?
C3 C8 C12 121.0(2) . . ?
C4 C9 C11 111.8(3) . . ?
C4 C9 C10 114.7(3) . . ?
C11 C9 C10 109.1(3) . . ?
C8 C12 C14 111.4(3) . . ?
C8 C12 C13 114.3(3) . . ?
C14 C12 C13 109.2(3) . . ?
C20 C15 C16 120.0(2) . . ?
C20 C15 N2 119.42(19) . . ?
C16 C15 N2 120.6(2) . . ?
C17 C16 C15 118.9(2) . . ?
C17 C16 C21 120.8(3) . . ?
C15 C16 C21 119.1(3) . . ?
C17 C16 C21A 118.4(3) . . ?
C15 C16 C21A 122.0(3) . . ?
C21 C16 C21A 19.8(3) . . ?
C18 C17 C16 121.4(2) . . ?
C17 C18 C19 119.5(2) . . ?
C18 C19 C20 121.4(2) . . ?
C19 C20 C15 118.8(2) . . ?
C19 C20 C24 120.8(2) . . ?
C15 C20 C24 120.4(2) . . ?
C16 C21 C23 103.0(6) . . ?
C16 C21 C22 115.5(6) . . ?
C23 C21 C22 109.1(6) . . ?
C26 C24 C20 113.5(2) . . ?
C26 C24 C25 110.6(3) . . ?
C20 C24 C25 111.3(3) . . ?
N3 C27 C28 116.0(4) . . ?
N4 C28 C27 118.0(3) . . ?
C23A C21A C22A 108.9(6) . . ?
C23A C21A C16 117.1(5) . . ?
C22A C21A C16 106.7(4) . . ?
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
Sm1 N3 2.700(2) . ?
Sm1 N3 2.700(2) 5 ?
Sm1 N4 2.748(3) 5 ?
Sm1 N4 2.748(3) . ?
Sm1 Ga1 3.3124(9) 5 ?
Sm1 Ga1 3.3124(9) . ?
Ga1 N1 1.9287(18) . ?
Ga1 N2 1.9326(18) . ?
N1 C1 1.389(3) . ?
N1 C3 1.424(3) . ?
C1 C2 1.345(3) . ?
N2 C2 1.390(3) . ?
N2 C15 1.420(3) . ?
N3 C29 1.406(4) . ?
N3 C30 1.468(5) . ?
N3 C27 1.469(7) . ?
C3 C4 1.398(4) . ?
C3 C8 1.410(4) . ?
N4 C32 1.436(5) . ?
N4 C28 1.458(5) . ?
N4 C31 1.463(5) . ?
C4 C5 1.403(4) . ?
C4 C9 1.506(5) . ?
C5 C6 1.355(6) . ?
C6 C7 1.369(6) . ?
C7 C8 1.401(4) . ?
C8 C12 1.524(5) . ?
C9 C11 1.507(6) . ?
C9 C10 1.529(4) . ?
C12 C14 1.526(4) . ?
C12 C13 1.539(5) . ?
C15 C20 1.399(3) . ?
C15 C16 1.407(3) . ?
C16 C17 1.393(3) . ?
C16 C21 1.467(8) . ?
C16 C21A 1.601(6) . ?
C17 C18 1.367(4) . ?
C18 C19 1.381(3) . ?
C19 C20 1.393(3) . ?
C20 C24 1.523(3) . ?
C21 C23 1.522(9) . ?
C21 C22 1.526(9) . ?
C23A C21A 1.514(8) . ?
C24 C26 1.519(5) . ?
C24 C25 1.528(5) . ?
C27 C28 1.467(8) . ?
C22A C21A 1.553(8) . ?
