#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/59/2205940.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205940
loop_
_publ_author_name
'Singh-Wilmot, Marvadeen A.'
'Kahwa, Ishenkumba A.'
'Lough, Alan J.'
_publ_section_title
Bis(μ-2,6-diformyl-4-methylphenolato)bis[bis(2,6-diformyl-4-methylphenolato)neodymium(III)]
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1009
_journal_page_last               m1011
_journal_paper_doi               10.1107/S160053680500591X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Nd2 (C9 H7 O3)6]'
_chemical_formula_moiety         'C54 H42 Nd2 O18'
_chemical_formula_sum            'C54 H42 Nd2 O18'
_chemical_formula_weight         1267.36
_chemical_name_systematic
;
Bis(μ-2,6-diformyl-4-methylphenolato)bis[bis(2,6-diformyl-4-
methylphenolato)neodymium(III)]
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.1810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.1211(6)
_cell_length_b                   15.0486(4)
_cell_length_c                   15.5611(5)
_cell_measurement_reflns_used    4265
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.6
_cell_volume                     4907.2(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2003)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL and PLATON (Spek, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_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  0.061
_diffrn_reflns_av_sigmaI/netI    0.082
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14613
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Cut needle'
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.677
_refine_ls_extinction_coef       0.00056(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0401
_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)+5.4862P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                3340
_reflns_number_total             4319
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6156.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2205940
_cod_database_fobs_code          2205940
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Nd1 0.092127(13) 0.470968(18) 0.041908(17) 0.03144(14) Uani d . 1 . . Nd
O1 0.0801(2) 0.5464(3) 0.1829(2) 0.0602(13) Uani d . 1 . . O
O2 0.00945(16) 0.5873(2) 0.0250(2) 0.0323(8) Uani d . 1 . . O
O3 -0.04991(17) 0.6585(3) -0.1289(2) 0.0388(9) Uani d . 1 . . O
O4 0.08639(18) 0.5078(2) -0.1148(2) 0.0399(9) Uani d . 1 . . O
O5 0.15521(17) 0.5925(2) 0.0266(2) 0.0379(9) Uani d . 1 . . O
O6 0.2129(3) 0.8250(4) 0.1363(3) 0.059(2) Uani d PD 0.794(14) A 1 O
O6A 0.1920(11) 0.7074(15) 0.1600(12) 0.073(10) Uani d PD 0.206(14) A 2 O
O7 0.18298(18) 0.4292(3) 0.1496(2) 0.0450(10) Uani d . 1 . . O
O8 0.13778(17) 0.3454(2) -0.0069(2) 0.0361(8) Uani d . 1 . . O
O9 0.1254(3) 0.1221(3) -0.1477(3) 0.0722(14) Uani d . 1 . . O
C1 0.0174(2) 0.6699(3) 0.0501(3) 0.0304(11) Uani d . 1 . . C
C2 0.0443(3) 0.6912(3) 0.1353(3) 0.0349(12) Uani d . 1 . . C
C3 0.0523(3) 0.7807(4) 0.1611(4) 0.0433(14) Uani d . 1 . . C
H3A 0.0684 0.7936 0.2195 0.052 Uiso calc R 1 . . H
C4 0.0375(3) 0.8505(4) 0.1038(4) 0.0465(15) Uani d . 1 . . C
C5 0.0122(3) 0.8285(4) 0.0217(4) 0.0432(14) Uani d . 1 . . C
H5A 0.0022 0.8755 -0.0185 0.052 Uiso calc R 1 . . H
C6 0.0001(3) 0.7419(3) -0.0075(3) 0.0344(12) Uani d . 1 . . C
C7 0.0657(3) 0.6219(4) 0.1984(4) 0.0470(15) Uani d . 1 . . C
H7A 0.0686 0.6380 0.2578 0.056 Uiso calc R 1 . . H
C8 -0.0270(3) 0.7277(4) -0.0960(3) 0.0367(13) Uani d . 1 . . C
H8A -0.0273 0.7775 -0.1334 0.044 Uiso calc R 1 . . H
C9 0.0485(4) 0.9458(4) 0.1342(5) 0.071(2) Uani d . 1 . . C
H9A 0.0718 0.9780 0.0933 0.106 Uiso calc R 1 . . H
H9B 0.0735 0.9462 0.1917 0.106 Uiso calc R 1 . . H
H9C 0.0073 0.9748 0.1373 0.106 Uiso calc R 1 . . H
C10 0.1506(3) 0.6618(4) -0.0226(4) 0.0358(12) Uani d . 1 . . C
C11 0.1231(3) 0.6577(3) -0.1121(3) 0.0352(12) Uani d . 1 . . C
C12 0.1209(3) 0.7347(4) -0.1642(4) 0.0438(14) Uani d . 1 . . C
H12A 0.1045 0.7301 -0.2237 0.053 Uiso calc R 1 . . H
C13 0.1417(3) 0.8168(4) -0.1316(4) 0.0493(15) Uani d . 1 . . C
C14 0.1663(3) 0.8204(4) -0.0447(4) 0.0485(15) Uani d . 1 . . C
H14A 0.1805 0.8761 -0.0208 0.058 Uiso calc R 1 . . H
C15 0.1712(3) 0.7466(4) 0.0091(3) 0.0363(13) Uani d . 1 . . C
C16 0.0962(3) 0.5781(4) -0.1510(3) 0.0370(12) Uani d . 1 . . C
H16A 0.0846 0.5796 -0.2119 0.044 Uiso calc R 1 . . H
C17 0.1980(3) 0.7562(5) 0.1005(4) 0.0494(15) Uani d D 1 A 1 C
H17A 0.2040 0.7034 0.1341 0.059 Uiso calc PR 0.794(14) A 1 H
H17B 0.2233 0.8076 0.1143 0.059 Uiso calc PR 0.206(14) A 2 H
C18 0.1364(4) 0.8983(5) -0.1877(5) 0.076(2) Uani d . 1 . . C
H18A 0.1779 0.9283 -0.1832 0.115 Uiso calc R 1 . . H
H18B 0.1046 0.9387 -0.1685 0.115 Uiso calc R 1 . . H
H18C 0.1233 0.8811 -0.2481 0.115 Uiso calc R 1 . . H
C19 0.1657(2) 0.2756(3) 0.0297(3) 0.0342(12) Uani d . 1 . . C
C20 0.2014(3) 0.2774(4) 0.1139(4) 0.0377(13) Uani d . 1 . . C
C21 0.2311(3) 0.1998(4) 0.1500(4) 0.0464(14) Uani d . 1 . . C
H21A 0.2550 0.2029 0.2058 0.056 Uiso calc R 1 . . H
C22 0.2266(3) 0.1187(4) 0.1069(4) 0.0442(14) Uani d . 1 . . C
C23 0.1926(3) 0.1178(4) 0.0248(4) 0.0450(14) Uani d . 1 . . C
H23A 0.1894 0.0632 -0.0062 0.054 Uiso calc R 1 . . H
C24 0.1630(3) 0.1925(4) -0.0148(4) 0.0383(13) Uani d . 1 . . C
C25 0.2099(3) 0.3571(4) 0.1647(4) 0.0442(14) Uani d . 1 . . C
H25A 0.2396 0.3540 0.2158 0.053 Uiso calc R 1 . . H
C26 0.1296(3) 0.1873(4) -0.1023(4) 0.0487(15) Uani d . 1 . . C
H26A 0.1092 0.2398 -0.1256 0.058 Uiso calc R 1 . . H
C27 0.2578(4) 0.0366(4) 0.1475(5) 0.0643(19) Uani d . 1 . . C
H27A 0.2925 0.0536 0.1923 0.096 Uiso calc R 1 . . H
H27B 0.2751 0.0011 0.1031 0.096 Uiso calc R 1 . . H
H27C 0.2262 0.0014 0.1737 0.096 Uiso calc R 1 . . H
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 Nd1 O8 . . 110.43(13) y
O5 Nd1 O2 . 5_565 137.49(11) y
O8 Nd1 O2 . 5_565 86.93(12) y
O5 Nd1 O2 . . 80.53(12) y
O8 Nd1 O2 . . 150.67(11) y
O2 Nd1 O2 5_565 . 68.52(13) y
O5 Nd1 O7 . . 82.02(13) y
O8 Nd1 O7 . . 72.01(13) y
O2 Nd1 O7 5_565 . 140.35(12) y
O2 Nd1 O7 . . 137.31(12) y
O5 Nd1 O4 . . 71.25(12) y
O8 Nd1 O4 . . 80.22(12) y
O2 Nd1 O4 5_565 . 74.23(12) y
O2 Nd1 O4 . . 77.88(11) y
O7 Nd1 O4 . . 131.38(13) y
O5 Nd1 O1 . . 81.59(14) y
O8 Nd1 O1 . . 138.96(12) y
O2 Nd1 O1 5_565 . 110.92(14) y
O2 Nd1 O1 . . 67.95(12) y
O7 Nd1 O1 . . 71.14(14) y
O4 Nd1 O1 . . 139.26(12) y
O5 Nd1 O3 . 5_565 153.59(11) y
O8 Nd1 O3 . 5_565 74.94(12) y
O2 Nd1 O3 5_565 5_565 67.03(11) y
O2 Nd1 O3 . 5_565 107.71(11) y
O7 Nd1 O3 . 5_565 75.08(12) y
O4 Nd1 O3 . 5_565 134.51(12) y
O1 Nd1 O3 . 5_565 78.71(13) y
O5 Nd1 Nd1 . 5_565 110.03(9) ?
O8 Nd1 Nd1 . 5_565 119.93(9) ?
O2 Nd1 Nd1 5_565 5_565 34.54(8) ?
O2 Nd1 Nd1 . 5_565 33.98(8) ?
O7 Nd1 Nd1 . 5_565 155.54(10) ?
O4 Nd1 Nd1 . 5_565 73.07(9) ?
O1 Nd1 Nd1 . 5_565 89.18(11) ?
O3 Nd1 Nd1 5_565 5_565 87.18(8) ?
C7 O1 Nd1 . . 130.9(4) ?
C1 O2 Nd1 . 5_565 123.0(3) ?
C1 O2 Nd1 . . 125.5(3) ?
Nd1 O2 Nd1 5_565 . 111.48(13) ?
C8 O3 Nd1 . 5_565 124.0(3) ?
C16 O4 Nd1 . . 130.6(3) ?
C10 O5 Nd1 . . 134.8(3) ?
C25 O7 Nd1 . . 130.9(4) ?
C19 O8 Nd1 . . 135.0(3) ?
O2 C1 C2 . . 121.2(4) ?
O2 C1 C6 . . 121.5(4) ?
C2 C1 C6 . . 117.4(5) ?
C3 C2 C1 . . 120.3(5) ?
C3 C2 C7 . . 118.3(5) ?
C1 C2 C7 . . 121.4(5) ?
C4 C3 C2 . . 122.1(5) ?
C4 C3 H3A . . 119.0 ?
C2 C3 H3A . . 119.0 ?
C5 C4 C3 . . 116.6(5) ?
C5 C4 C9 . . 123.3(6) ?
C3 C4 C9 . . 120.1(6) ?
C4 C5 C6 . . 124.6(5) ?
C4 C5 H5A . . 117.7 ?
C6 C5 H5A . . 117.7 ?
C5 C6 C1 . . 118.9(5) ?
C5 C6 C8 . . 119.1(5) ?
C1 C6 C8 . . 121.9(5) ?
O1 C7 C2 . . 126.9(5) ?
O1 C7 H7A . . 116.6 ?
C2 C7 H7A . . 116.6 ?
O3 C8 C6 . . 127.8(5) ?
O3 C8 H8A . . 116.1 ?
C6 C8 H8A . . 116.1 ?
C4 C9 H9A . . 109.5 ?
C4 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C4 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
O5 C10 C15 . . 121.6(5) ?
O5 C10 C11 . . 122.0(5) ?
C15 C10 C11 . . 116.4(5) ?
C12 C11 C16 . . 117.6(5) ?
C12 C11 C10 . . 120.0(5) ?
C16 C11 C10 . . 122.4(5) ?
C13 C12 C11 . . 122.4(5) ?
C13 C12 H12A . . 118.8 ?
C11 C12 H12A . . 118.8 ?
C12 C13 C14 . . 117.0(5) ?
C12 C13 C18 . . 121.2(6) ?
C14 C13 C18 . . 121.8(6) ?
C15 C14 C13 . . 123.2(5) ?
C15 C14 H14A . . 118.4 ?
C13 C14 H14A . . 118.4 ?
C14 C15 C10 . . 121.0(5) ?
C14 C15 C17 . . 119.7(5) ?
C10 C15 C17 . . 119.3(5) ?
O4 C16 C11 . . 127.6(5) ?
O4 C16 H16A . . 116.2 ?
C11 C16 H16A . . 116.2 ?
O6 C17 C15 . . 125.5(7) ?
O6 C17 H17A . . 117.3 ?
C15 C17 H17A . . 117.3 ?
C13 C18 H18A . . 109.5 ?
C13 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C13 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
O8 C19 C20 . . 123.0(5) ?
O8 C19 C24 . . 120.4(5) ?
C20 C19 C24 . . 116.5(5) ?
C21 C20 C19 . . 120.5(5) ?
C21 C20 C25 . . 117.0(5) ?
C19 C20 C25 . . 122.4(5) ?
C22 C21 C20 . . 122.4(5) ?
C22 C21 H21A . . 118.8 ?
C20 C21 H21A . . 118.8 ?
C23 C22 C21 . . 116.7(5) ?
C23 C22 C27 . . 121.9(6) ?
C21 C22 C27 . . 121.3(6) ?
C22 C23 C24 . . 123.5(6) ?
C22 C23 H23A . . 118.2 ?
C24 C23 H23A . . 118.2 ?
C23 C24 C19 . . 120.3(5) ?
C23 C24 C26 . . 120.6(5) ?
C19 C24 C26 . . 119.1(5) ?
O7 C25 C20 . . 127.3(5) ?
O7 C25 H25A . . 116.3 ?
C20 C25 H25A . . 116.3 ?
O9 C26 C24 . . 125.7(6) ?
O9 C26 H26A . . 117.2 ?
C24 C26 H26A . . 117.2 ?
C22 C27 H27A . . 109.5 ?
C22 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C22 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Nd1 O5 . 2.293(4) y
Nd1 O8 . 2.293(3) y
Nd1 O2 5_565 2.428(3) y
Nd1 O2 . 2.463(3) y
Nd1 O7 . 2.466(3) y
Nd1 O4 . 2.489(4) y
Nd1 O1 . 2.511(4) y
Nd1 O3 5_565 2.593(4) y
Nd1 Nd1 5_565 4.0424(5) n
O1 C7 . 1.208(7) ?
O2 C1 . 1.309(6) ?
O2 Nd1 5_565 2.428(3) ?
O3 C8 . 1.232(6) ?
O3 Nd1 5_565 2.593(4) ?
O4 C16 . 1.228(6) ?
O5 C10 . 1.291(6) ?
O6 C17 . 1.199(7) ?
O7 C25 . 1.233(7) ?
O8 C19 . 1.300(6) ?
O9 C26 . 1.207(7) ?
C1 C2 . 1.413(7) ?
C1 C6 . 1.425(7) ?
C2 C3 . 1.409(7) ?
C2 C7 . 1.465(8) ?
C3 C4 . 1.388(8) ?
C3 H3A . 0.9500 ?
C4 C5 . 1.363(8) ?
C4 C9 . 1.518(8) ?
C5 C6 . 1.392(7) ?
C5 H5A . 0.9500 ?
C6 C8 . 1.440(7) ?
C7 H7A . 0.9500 ?
C8 H8A . 0.9500 ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
C10 C15 . 1.417(7) ?
C10 C11 . 1.442(8) ?
C11 C12 . 1.411(8) ?
C11 C16 . 1.428(8) ?
C12 C13 . 1.387(8) ?
C12 H12A . 0.9500 ?
C13 C14 . 1.389(9) ?
C13 C18 . 1.502(8) ?
C14 C15 . 1.386(8) ?
C14 H14A . 0.9500 ?
C15 C17 . 1.471(8) ?
C16 H16A . 0.9500 ?
C17 H17A . 0.9500 ?
C18 H18A . 0.9800 ?
C18 H18B . 0.9800 ?
C18 H18C . 0.9800 ?
C19 C20 . 1.428(8) ?
C19 C24 . 1.428(8) ?
C20 C21 . 1.409(8) ?
C20 C25 . 1.436(8) ?
C21 C22 . 1.389(8) ?
C21 H21A . 0.9500 ?
C22 C23 . 1.386(8) ?
C22 C27 . 1.503(8) ?
C23 C24 . 1.393(8) ?
C23 H23A . 0.9500 ?
C24 C26 . 1.455(8) ?
C25 H25A . 0.9500 ?
C26 H26A . 0.9500 ?
C27 H27A . 0.9800 ?
C27 H27B . 0.9800 ?
C27 H27C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C3 H3A O9 6_566 0.95 2.59 3.497(7) 160
C16 H16A O1 6_565 0.95 2.50 3.176(6) 128
C25 H25A O6 4_545 0.95 2.43 3.349(8) 162
