#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/48/7204829.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_7204829
loop_
_publ_author_name
'Carsten P. Roll'
'Alexander G. Martin'
'Helmar Görls'
'Guido Leibeling'
'Daniel Guillon'
'Bertrand Donnio'
'Wolfgang Weigand'
_publ_section_title
;
 Rodlike metallomesogens containing nickel(II), palladium(II) and
 copper(II) based on novel enaminoketonato ligands
;
_journal_issue                   11
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              1722
_journal_page_last               1730
_journal_paper_doi               10.1039/b316731c
_journal_volume                  14
_journal_year                    2004
_chemical_formula_sum            'C28 H37 N O4'
_chemical_formula_weight         451.59
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.927(7)
_cell_angle_beta                 93.548(6)
_cell_angle_gamma                91.903(7)
_cell_formula_units_Z            2
_cell_length_a                   5.1776(4)
_cell_length_b                   11.785(1)
_cell_length_c                   20.724(2)
_cell_measurement_temperature    183(2)
_cell_volume                     1260.61(19)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4-EXPRESS
_computing_data_reduction        MOLEN
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       omega-2theta-scan
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6389
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        -0.22
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9860
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.706
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.706
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0100P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                3193
_reflns_number_total             5749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316731c.txt
_cod_data_source_block           FO1388
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom/difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1260.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204829
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 1.2861(5) -0.27157(19) 0.13952(11) 0.0468(7) Uani 1 1 d . . .
O2 O 0.3771(5) 0.24906(18) 0.21237(10) 0.0399(7) Uani 1 1 d . . .
O3 O 0.2535(5) 0.32248(18) 0.11651(10) 0.0371(6) Uani 1 1 d . . .
O4 O -0.3880(5) 0.58966(19) 0.32273(10) 0.0384(7) Uani 1 1 d . . .
N1 N 0.9300(6) -0.1148(2) 0.11885(13) 0.0383(8) Uani 1 1 d . . .
C1 C 1.3701(8) -0.4045(3) 0.05484(17) 0.0446(11) Uani 1 1 d . . .
H1A H 1.5007 -0.4299 0.0870 0.067 Uiso 1 1 calc R . .
H1B H 1.4550 -0.3799 0.0165 0.067 Uiso 1 1 calc R . .
H1C H 1.2463 -0.4674 0.0426 0.067 Uiso 1 1 calc R . .
C2 C 1.2288(7) -0.3066(3) 0.08339(16) 0.0338(9) Uani 1 1 d . . .
C3 C 1.0291(7) -0.2584(3) 0.04254(15) 0.0298(8) Uani 1 1 d . . .
H3A H 0.9909 -0.2923 0.0007 0.036 Uiso 1 1 calc R . .
C4 C 0.8914(7) -0.1671(3) 0.06027(15) 0.0316(9) Uani 1 1 d . . .
C5 C 0.6848(7) -0.1220(3) 0.01503(15) 0.0380(9) Uani 1 1 d . . .
H5A H 0.6073 -0.0566 0.0359 0.057 Uiso 1 1 calc R . .
H5B H 0.5508 -0.1815 0.0044 0.057 Uiso 1 1 calc R . .
H5C H 0.7613 -0.0984 -0.0247 0.057 Uiso 1 1 calc R . .
C6 C 0.7896(7) -0.0194(3) 0.14116(15) 0.0315(9) Uani 1 1 d . . .
C7 C 0.6090(8) -0.0350(3) 0.18595(16) 0.0432(10) Uani 1 1 d . . .
H7A H 0.5781 -0.1084 0.2020 0.052 Uiso 1 1 calc R . .
C8 C 0.4718(8) 0.0554(3) 0.20783(16) 0.0446(11) Uani 1 1 d . . .
H8A H 0.3477 0.0444 0.2391 0.054 Uiso 1 1 calc R . .
C9 C 0.5152(7) 0.1610(3) 0.18428(15) 0.0316(9) Uani 1 1 d . . .
C10 C 0.6946(7) 0.1784(3) 0.13929(16) 0.0374(9) Uani 1 1 d . . .
H10A H 0.7234 0.2515 0.1226 0.045 Uiso 1 1 calc R . .
C11 C 0.8323(7) 0.0869(3) 0.11882(17) 0.0410(10) Uani 1 1 d . . .
H11A H 0.9599 0.0982 0.0884 0.049 Uiso 1 1 calc R . .
C12 C 0.2435(7) 0.3223(3) 0.17434(16) 0.0316(9) Uani 1 1 d . . .
C13 C 0.0847(7) 0.3956(3) 0.21357(15) 0.0288(8) Uani 1 1 d . . .
C14 C 0.0806(7) 0.3876(3) 0.28033(15) 0.0368(10) Uani 1 1 d . . .
H14A H 0.1898 0.3361 0.3021 0.044 Uiso 1 1 calc R . .
C15 C -0.0780(7) 0.4528(3) 0.31479(15) 0.0386(10) Uani 1 1 d . . .
H15A H -0.0787 0.4463 0.3603 0.046 Uiso 1 1 calc R . .
C16 C -0.2400(7) 0.5292(3) 0.28356(15) 0.0297(8) Uani 1 1 d . . .
C17 C -0.2400(7) 0.5387(3) 0.21713(15) 0.0312(9) Uani 1 1 d . . .
H17A H -0.3498 0.5901 0.1954 0.037 Uiso 1 1 calc R . .
C18 C -0.0759(7) 0.4714(3) 0.18283(15) 0.0305(9) Uani 1 1 d . . .
H18A H -0.0740 0.4777 0.1373 0.037 Uiso 1 1 calc R . .
C19 C -0.5607(7) 0.6706(3) 0.29386(15) 0.0329(9) Uani 1 1 d . . .
H19A H -0.6954 0.6308 0.2647 0.039 Uiso 1 1 calc R . .
H19B H -0.4630 0.7251 0.2684 0.039 Uiso 1 1 calc R . .
C20 C -0.6823(7) 0.7317(3) 0.34788(15) 0.0352(9) Uani 1 1 d . . .
H20A H -0.5438 0.7650 0.3786 0.042 Uiso 1 1 calc R . .
H20B H -0.7851 0.6762 0.3714 0.042 Uiso 1 1 calc R . .
C21 C -0.8567(7) 0.8254(3) 0.32530(15) 0.0333(9) Uani 1 1 d . . .
H21A H -0.7596 0.8762 0.2976 0.040 Uiso 1 1 calc R . .
H21B H -1.0064 0.7911 0.2987 0.040 Uiso 1 1 calc R . .
C22 C -0.9551(7) 0.8952(3) 0.38068(16) 0.0382(9) Uani 1 1 d . . .
H22A H -0.8041 0.9278 0.4075 0.046 Uiso 1 1 calc R . .
H22B H -1.0521 0.8437 0.4081 0.046 Uiso 1 1 calc R . .
C23 C -1.1281(8) 0.9911(3) 0.36127(16) 0.0413(10) Uani 1 1 d . . .
H23A H -1.0327 1.0426 0.3336 0.050 Uiso 1 1 calc R . .
H23B H -1.2814 0.9589 0.3352 0.050 Uiso 1 1 calc R . .
C24 C -1.2189(7) 1.0595(3) 0.41786(16) 0.0430(10) Uani 1 1 d . . .
H24A H -1.3129 1.0075 0.4455 0.052 Uiso 1 1 calc R . .
H24B H -1.0648 1.0913 0.4439 0.052 Uiso 1 1 calc R . .
C25 C -1.3914(8) 1.1554(3) 0.40063(16) 0.0436(10) Uani 1 1 d . . .
H25A H -1.5468 1.1241 0.3750 0.052 Uiso 1 1 calc R . .
H25B H -1.2983 1.2078 0.3730 0.052 Uiso 1 1 calc R . .
C26 C -1.4777(8) 1.2224(3) 0.45929(17) 0.0486(11) Uani 1 1 d . . .
H26A H -1.5695 1.1694 0.4869 0.058 Uiso 1 1 calc R . .
H26B H -1.3216 1.2532 0.4848 0.058 Uiso 1 1 calc R . .
C27 C -1.6496(8) 1.3181(3) 0.44416(17) 0.0502(11) Uani 1 1 d . . .
H27A H -1.8038 1.2882 0.4175 0.060 Uiso 1 1 calc R . .
H27B H -1.5562 1.3731 0.4181 0.060 Uiso 1 1 calc R . .
C28 C -1.7378(9) 1.3796(3) 0.50373(18) 0.0678(14) Uani 1 1 d . . .
H28A H -1.8494 1.4414 0.4906 0.102 Uiso 1 1 calc R . .
H28B H -1.5864 1.4110 0.5299 0.102 Uiso 1 1 calc R . .
H28C H -1.8346 1.3262 0.5292 0.102 Uiso 1 1 calc R . .
H1N1 H 1.062(7) -0.150(3) 0.1491(16) 0.057(11) Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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
C12 O2 C9 120.5(2) . . ?
C16 O4 C19 118.4(2) . . ?
C4 N1 C6 125.1(3) . . ?
O1 C2 C3 123.0(3) . . ?
O1 C2 C1 120.0(3) . . ?
C3 C2 C1 117.0(3) . . ?
C4 C3 C2 124.0(3) . . ?
N1 C4 C3 122.0(3) . . ?
N1 C4 C5 117.0(3) . . ?
C3 C4 C5 120.9(3) . . ?
C11 C6 C7 119.0(3) . . ?
C11 C6 N1 121.5(3) . . ?
C7 C6 N1 119.5(3) . . ?
C6 C7 C8 120.4(3) . . ?
C9 C8 C7 119.7(4) . . ?
C8 C9 C10 120.8(3) . . ?
C8 C9 O2 115.5(3) . . ?
C10 C9 O2 123.5(3) . . ?
C9 C10 C11 118.4(3) . . ?
C6 C11 C10 121.7(4) . . ?
O3 C12 O2 123.1(3) . . ?
O3 C12 C13 126.2(3) . . ?
O2 C12 C13 110.7(3) . . ?
C18 C13 C14 118.6(3) . . ?
C18 C13 C12 119.0(3) . . ?
C14 C13 C12 122.3(3) . . ?
C15 C14 C13 120.8(3) . . ?
C14 C15 C16 120.4(3) . . ?
O4 C16 C17 124.8(3) . . ?
O4 C16 C15 115.2(3) . . ?
C17 C16 C15 120.0(3) . . ?
C16 C17 C18 118.7(3) . . ?
C13 C18 C17 121.5(3) . . ?
O4 C19 C20 107.2(2) . . ?
C19 C20 C21 113.3(3) . . ?
C22 C21 C20 112.9(3) . . ?
C21 C22 C23 115.5(3) . . ?
C24 C23 C22 113.8(3) . . ?
C25 C24 C23 115.4(3) . . ?
C24 C25 C26 113.6(3) . . ?
C27 C26 C25 115.2(3) . . ?
C26 C27 C28 113.4(3) . . ?
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
O1 C2 1.236(4) . ?
O2 C12 1.365(4) . ?
O2 C9 1.410(4) . ?
O3 C12 1.203(3) . ?
O4 C16 1.352(4) . ?
O4 C19 1.448(4) . ?
N1 C4 1.343(4) . ?
N1 C6 1.438(4) . ?
C1 C2 1.510(4) . ?
C2 C3 1.439(4) . ?
C3 C4 1.363(4) . ?
C4 C5 1.501(4) . ?
C6 C11 1.366(4) . ?
C6 C7 1.370(5) . ?
C7 C8 1.379(5) . ?
C8 C9 1.369(4) . ?
C9 C10 1.371(4) . ?
C10 C11 1.382(4) . ?
C12 C13 1.471(4) . ?
C13 C18 1.385(4) . ?
C13 C14 1.391(4) . ?
C14 C15 1.361(4) . ?
C15 C16 1.398(4) . ?
C16 C17 1.385(4) . ?
C17 C18 1.392(4) . ?
C19 C20 1.493(4) . ?
C20 C21 1.518(4) . ?
C21 C22 1.513(4) . ?
C22 C23 1.515(4) . ?
C23 C24 1.508(4) . ?
C24 C25 1.502(4) . ?
C25 C26 1.526(4) . ?
C26 C27 1.489(5) . ?
C27 C28 1.513(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30653717
