#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:41:02 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180049 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/43/7034352.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_7034352
loop_
_publ_author_name
'Zaragoza-Calero, Silvia'
'Francos, Javier'
'Kennedy, Alan R.'
'O'Hara, Charles T'
_publ_section_title
;
 Solid state and solution studies of lithium tris(n-butyl)magnesiates
 stabilised by Lewis donors.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7258
_journal_page_last               7267
_journal_paper_doi               10.1039/c5dt00435g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C19 H38 Li Mg O2'
_chemical_formula_weight         329.74
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_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
_audit_update_record
;
2015-01-28 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.437(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.5458(8)
_cell_length_b                   22.265(2)
_cell_length_c                   18.0116(12)
_cell_measurement_reflns_used    3607
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.8008
_cell_measurement_theta_min      3.0255
_cell_volume                     4221.6(6)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_publication_material  'SHELXL-97 '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       '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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11951
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0924
_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)+(0.1320P)²+7.9697P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2420
_refine_ls_wR_factor_ref         0.2721
_reflns_number_gt                2704
_reflns_number_total             4082
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c5dt00435g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7034348--7034352.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7034352
#BEGIN Tags that were not found in dictionaries:
_cell_oxdiff_measurement_reflns_used 3608
#END Tags that were not found in dictionaries
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
Mg1 Mg 0.03209(11) 0.05606(6) 0.02789(6) 0.0417(4) Uani 1 1 d . . .
Li1 Li 0.0936(6) 0.1577(3) 0.0882(3) 0.0430(14) Uani 1 1 d U . .
O1 O 0.1582(2) 0.23182(11) 0.04931(13) 0.0421(6) Uani 1 1 d . . .
O2 O 0.0905(3) 0.16997(13) 0.19570(14) 0.0590(8) Uani 1 1 d U . .
C1 C 0.2270(4) 0.08221(19) 0.0702(2) 0.0563(11) Uani 1 1 d DU . .
H1A H 0.2693 0.1077 0.0341 0.068 Uiso 1 1 calc R A 1
H1B H 0.2260 0.1035 0.1185 0.068 Uiso 1 1 calc R A 1
C2 C 0.2895(9) 0.0213(4) 0.0787(7) 0.085(3) Uani 0.681(7) 1 d PDU B 1
H2A H 0.2433 -0.0019 0.1153 0.102 Uiso 0.681(7) 1 calc PR B 1
H2B H 0.2777 0.0002 0.0304 0.102 Uiso 0.681(7) 1 calc PR B 1
C3 C 0.4279(9) 0.0197(5) 0.1024(10) 0.152(4) Uani 0.681(7) 1 d PDU B 1
H3A H 0.4332 0.0129 0.1568 0.183 Uiso 0.681(7) 1 calc PR B 1
H3B H 0.4627 -0.0169 0.0798 0.183 Uiso 0.681(7) 1 calc PR B 1
C4 C 0.5163(11) 0.0683(6) 0.0886(12) 0.193(5) Uani 0.681(7) 1 d PDU B 1
H4A H 0.6034 0.0549 0.1012 0.289 Uiso 0.681(7) 1 calc PR B 1
H4B H 0.4971 0.1030 0.1194 0.289 Uiso 0.681(7) 1 calc PR B 1
H4C H 0.5077 0.0797 0.0360 0.289 Uiso 0.681(7) 1 calc PR B 1
C5 C 0.0396(4) 0.02565(19) -0.0927(2) 0.0517(10) Uani 1 1 d DU . .
H5A H 0.0056 -0.0157 -0.0972 0.062 Uiso 1 1 calc R B 1
H5B H -0.0166 0.0520 -0.1244 0.062 Uiso 1 1 calc R B 1
C6 C 0.1706(6) 0.0266(4) -0.1217(4) 0.0576(18) Uani 0.681(7) 1 d PDU B 1
H6A H 0.1976 -0.0153 -0.1301 0.069 Uiso 0.681(7) 1 calc PR B 1
H6B H 0.2302 0.0440 -0.0830 0.069 Uiso 0.681(7) 1 calc PR B 1
C7 C 0.1823(13) 0.0621(6) -0.1942(6) 0.076(2) Uani 0.681(7) 1 d PDU B 1
H7A H 0.1311 0.0418 -0.2347 0.091 Uiso 0.681(7) 1 calc PR B 1
H7B H 0.1465 0.1028 -0.1880 0.091 Uiso 0.681(7) 1 calc PR B 1
C8 C 0.3189(9) 0.0678(6) -0.2166(6) 0.105(3) Uani 0.681(7) 1 d PDU B 1
H8A H 0.3206 0.0917 -0.2622 0.158 Uiso 0.681(7) 1 calc PR B 1
H8B H 0.3536 0.0278 -0.2253 0.158 Uiso 0.681(7) 1 calc PR B 1
H8C H 0.3703 0.0877 -0.1767 0.158 Uiso 0.681(7) 1 calc PR B 1
C9 C 0.0660(6) 0.1180(2) 0.2391(3) 0.0896(18) Uani 1 1 d U . .
H9A H 0.1244 0.1176 0.2843 0.108 Uiso 1 1 calc R . .
H9B H 0.0818 0.0814 0.2100 0.108 Uiso 1 1 calc R . .
C10 C 0.0666(4) 0.22224(18) 0.2379(2) 0.0466(9) Uani 1 1 d U . .
H10A H 0.0803 0.2584 0.2074 0.056 Uiso 1 1 calc R . .
H10B H 0.1269 0.2238 0.2821 0.056 Uiso 1 1 calc R . .
C11 C -0.1036(3) 0.13165(18) 0.0421(2) 0.0487(9) Uani 1 1 d . . .
H11A H -0.1558 0.1234 0.0849 0.058 Uiso 1 1 calc R B .
H11B H -0.0561 0.1694 0.0521 0.058 Uiso 1 1 calc R . .
C12 C -0.1882(4) 0.1381(2) -0.0278(2) 0.0545(11) Uani 1 1 d . B .
H12A H -0.1419 0.1626 -0.0632 0.065 Uiso 1 1 calc R . .
H12B H -0.1995 0.0977 -0.0500 0.065 Uiso 1 1 calc R . .
C13 C -0.3171(4) 0.1651(2) -0.0231(3) 0.0696(13) Uani 1 1 d . . .
H13A H -0.3640 0.1411 0.0126 0.084 Uiso 1 1 calc R B .
H13B H -0.3068 0.2061 -0.0023 0.084 Uiso 1 1 calc R . .
C14 C -0.3961(5) 0.1692(3) -0.0933(3) 0.0793(16) Uani 1 1 d . B .
H14A H -0.3489 0.1903 -0.1306 0.119 Uiso 1 1 calc R . .
H14B H -0.4743 0.1912 -0.0848 0.119 Uiso 1 1 calc R . .
H14C H -0.4176 0.1286 -0.1113 0.119 Uiso 1 1 calc R . .
C15 C 0.2746(3) 0.26003(19) 0.0762(2) 0.0480(10) Uani 1 1 d . . .
H15A H 0.2999 0.2447 0.1266 0.058 Uiso 1 1 calc R . .
H15B H 0.2618 0.3040 0.0797 0.058 Uiso 1 1 calc R . .
C16 C 0.1221(3) 0.2531(2) -0.0243(2) 0.0498(10) Uani 1 1 d . . .
H16A H 0.1064 0.2969 -0.0229 0.060 Uiso 1 1 calc R . .
H16B H 0.0424 0.2331 -0.0428 0.060 Uiso 1 1 calc R . .
C17 C 0.5426(6) 0.2886(3) 0.2228(3) 0.0938(19) Uani 1 1 d . . .
H17 H 0.5727 0.3256 0.2042 0.113 Uiso 1 1 calc R . .
C18 C 0.5430(8) 0.1847(4) 0.2230(6) 0.149(4) Uani 1 1 d . . .
H18 H 0.5740 0.1477 0.2050 0.178 Uiso 1 1 calc R . .
C19 C 0.5833(5) 0.2366(4) 0.1956(4) 0.103(2) Uani 1 1 d . . .
H19 H 0.6407 0.2366 0.1570 0.123 Uiso 1 1 calc R . .
C2A C 0.309(2) 0.0323(8) 0.1051(16) 0.085(3) Uani 0.319(7) 1 d PDU B 2
H2A1 H 0.3221 0.0027 0.0654 0.102 Uiso 0.319(7) 1 calc PR B 2
H2A2 H 0.2574 0.0120 0.1419 0.102 Uiso 0.319(7) 1 calc PR B 2
C3A C 0.440(2) 0.0447(12) 0.144(2) 0.152(4) Uani 0.319(7) 1 d PDU B 2
H3A1 H 0.4682 0.0854 0.1310 0.183 Uiso 0.319(7) 1 calc PR B 2
H3A2 H 0.4330 0.0431 0.1987 0.183 Uiso 0.319(7) 1 calc PR B 2
C4A C 0.538(2) -0.0015(13) 0.121(2) 0.193(5) Uani 0.319(7) 1 d PDU B 2
H4A1 H 0.6196 0.0069 0.1478 0.289 Uiso 0.319(7) 1 calc PR B 2
H4A2 H 0.5466 0.0011 0.0677 0.289 Uiso 0.319(7) 1 calc PR B 2
H4A3 H 0.5092 -0.0419 0.1342 0.289 Uiso 0.319(7) 1 calc PR B 2
C6A C 0.1514(14) 0.0589(8) -0.1188(9) 0.0576(18) Uani 0.319(7) 1 d PDU B 2
H6A1 H 0.2257 0.0482 -0.0851 0.069 Uiso 0.319(7) 1 calc PR B 2
H6A2 H 0.1353 0.1022 -0.1119 0.069 Uiso 0.319(7) 1 calc PR B 2
C7A C 0.190(3) 0.0501(12) -0.1987(12) 0.076(2) Uani 0.319(7) 1 d PDU B 2
H7A1 H 0.2375 0.0120 -0.2028 0.091 Uiso 0.319(7) 1 calc PR B 2
H7A2 H 0.1138 0.0484 -0.2333 0.091 Uiso 0.319(7) 1 calc PR B 2
C8A C 0.274(2) 0.1030(12) -0.2185(15) 0.105(3) Uani 0.319(7) 1 d PDU B 2
H8A1 H 0.3056 0.0966 -0.2679 0.158 Uiso 0.319(7) 1 calc PR B 2
H8A2 H 0.3461 0.1061 -0.1817 0.158 Uiso 0.319(7) 1 calc PR B 2
H8A3 H 0.2243 0.1402 -0.2184 0.158 Uiso 0.319(7) 1 calc PR B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
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'
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
C1 Mg1 C11 110.39(15) . .
C1 Mg1 C5 108.66(15) . .
C11 Mg1 C5 113.05(16) . .
C1 Mg1 C5 110.84(16) . 5
C11 Mg1 C5 107.69(15) . 5
C5 Mg1 C5 106.14(12) . 5
C1 Mg1 Li1 54.69(17) . .
C11 Mg1 Li1 55.72(17) . .
C5 Mg1 Li1 129.78(17) . .
C5 Mg1 Li1 124.06(17) 5 .
C1 Mg1 Mg1 124.22(12) . 5
C11 Mg1 Mg1 125.33(12) . 5
C5 Mg1 Mg1 53.60(11) . 5
C5 Mg1 Mg1 52.55(10) 5 5
Li1 Mg1 Mg1 176.40(15) . 5
O1 Li1 O2 105.4(3) . .
O1 Li1 Mg1 133.1(3) . .
O2 Li1 Mg1 121.4(3) . .
C15 O1 C16 110.0(3) . .
C15 O1 Li1 124.3(3) . .
C16 O1 Li1 122.3(3) . .
C10 O2 C9 109.1(3) . .
C10 O2 Li1 131.1(3) . .
C9 O2 Li1 116.3(3) . .
C2 C1 C2A 21.4(11) . .
C2 C1 Mg1 100.9(4) . .
C2A C1 Mg1 116.1(9) . .
C3 C2 C1 117.6(8) . .
C4 C3 C2 123.7(11) . .
C6A C5 C6 28.9(6) . .
C6A C5 Mg1 103.1(6) . .
C6 C5 Mg1 114.3(4) . .
C5 C6 C7 115.1(7) . .
C8 C7 C6 113.2(10) . .
O2 C9 C9 110.6(4) . 2
O2 C10 C10 110.9(3) . 2
C12 C11 Mg1 109.2(3) . .
C13 C12 C11 119.1(4) . .
C14 C13 C12 116.4(4) . .
O1 C15 C16 109.9(3) . 7
O1 C16 C15 110.3(3) . 7
C19 C17 C17 120.0(4) . 2_655
C19 C18 C18 120.1(5) . 2_655
C17 C19 C18 119.9(8) . .
C1 C2A C3A 122.1(17) . .
C4A C3A C2A 111(2) . .
C5 C6A C7A 119.6(13) . .
C8A C7A C6A 108.2(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 C1 2.226(4) .
Mg1 C11 2.234(4) .
Mg1 C5 2.281(4) .
Mg1 C5 2.313(4) 5
Mg1 Li1 2.576(6) .
Mg1 Mg1 2.760(2) 5
Li1 O1 1.933(7) .
Li1 O2 1.958(6) .
O1 C15 1.437(4) .
O1 C16 1.438(4) .
O2 C10 1.420(4) .
O2 C9 1.428(5) .
C1 C2 1.511(7) .
C1 C2A 1.520(10) .
C2 C3 1.496(8) .
C3 C4 1.460(9) .
C5 C6A 1.492(9) .
C5 C6 1.507(6) .
C6 C7 1.536(9) .
C7 C8 1.525(9) .
C9 C9 1.468(12) 2
C10 C10 1.496(7) 2
C11 C12 1.506(5) .
C12 C13 1.493(6) .
C13 C14 1.475(6) .
C15 C16 1.506(5) 7
C16 C15 1.506(5) 7
C17 C19 1.337(9) .
C17 C17 1.369(12) 2_655
C18 C19 1.337(10) .
C18 C18 1.37(2) 2_655
C2A C3A 1.535(10) .
C3A C4A 1.529(10) .
C6A C7A 1.531(10) .
C7A C8A 1.527(10) .
