#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/17/7221779.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_7221779
loop_
_publ_author_name
'Chen, Peng'
'Li, Hongfeng'
'Sun, Wenbin'
'Tang, Jinkui'
'Zhang, Lei'
'Yan, Pengfei'
_publ_section_title
;
 Crystallization of triple- and quadruple-stranded dinuclear
 bis-β-diketonate-Dy(iii) helicates: single molecule magnetic behavior
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7227
_journal_paper_doi               10.1039/C5CE01067E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C17 H17 N O2'
_chemical_formula_weight         267.32
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-01 deposited with the CCDC.
2015-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                94.615(7)
_cell_angle_beta                 98.690(7)
_cell_angle_gamma                99.967(7)
_cell_formula_units_Z            2
_cell_length_a                   8.2376(6)
_cell_length_b                   8.5362(7)
_cell_length_c                   10.4219(9)
_cell_measurement_reflns_used    5518
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      3.30
_cell_volume                     709.21(10)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5518
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.129
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0476
_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)+(0.0498P)²+0.0785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                2182
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01067e2.cif
_cod_data_source_block           1054124
_cod_depositor_comments
'Adding full bibliography for 7221777--7221779.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7221779
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
N1 N 0.17768(15) 0.86330(16) 0.24493(13) 0.0533(4) Uani 1 1 d .
C1 C 0.7033(2) 1.4136(2) 0.02989(18) 0.0654(5) Uani 1 1 d .
H1A H 0.8045 1.4591 0.0008 0.098 Uiso 1 1 calc R
H1B H 0.6736 1.4913 0.0896 0.098 Uiso 1 1 calc R
H1C H 0.6149 1.3830 -0.0439 0.098 Uiso 1 1 calc R
C2 C 0.7294(2) 1.26919(19) 0.09732(16) 0.0535(4) Uani 1 1 d .
C3 C 0.58430(18) 1.16833(17) 0.13715(14) 0.0455(4) Uani 1 1 d .
C4 C 0.42505(19) 1.20548(19) 0.12320(16) 0.0524(4) Uani 1 1 d .
H4A H 0.4077 1.2992 0.0881 0.063 Uiso 1 1 calc R
C5 C 0.29246(19) 1.10793(19) 0.15972(16) 0.0529(4) Uani 1 1 d .
H5A H 0.1878 1.1368 0.1490 0.064 Uiso 1 1 calc R
C6 C 0.31312(17) 0.96599(18) 0.21278(14) 0.0449(4) Uani 1 1 d .
C7 C 0.47375(18) 0.92790(18) 0.22762(15) 0.0484(4) Uani 1 1 d .
H7A H 0.4919 0.8344 0.2628 0.058 Uiso 1 1 calc R
C8 C 0.60393(18) 1.02715(18) 0.19073(15) 0.0496(4) Uani 1 1 d .
H8A H 0.7090 0.9992 0.2019 0.059 Uiso 1 1 calc R
C9 C 0.01024(19) 0.8652(3) 0.1768(2) 0.0736(6) Uani 1 1 d .
H9A H -0.0142 0.9706 0.1906 0.110 Uiso 1 1 calc R
H9B H -0.0697 0.7901 0.2099 0.110 Uiso 1 1 calc R
H9C H 0.0043 0.8362 0.0851 0.110 Uiso 1 1 calc R
C10 C 0.30656(19) 0.76858(19) 0.44362(15) 0.0511(4) Uani 1 1 d .
H10A H 0.3654 0.8718 0.4720 0.061 Uiso 1 1 calc R
C11 C 0.20031(18) 0.73778(18) 0.32317(15) 0.0465(4) Uani 1 1 d .
C12 C 0.11281(19) 0.58383(19) 0.28427(16) 0.0538(4) Uani 1 1 d .
H12A H 0.0403 0.5617 0.2048 0.065 Uiso 1 1 calc R
C13 C 0.1318(2) 0.46233(19) 0.36214(16) 0.0542(4) Uani 1 1 d .
H13A H 0.0721 0.3594 0.3340 0.065 Uiso 1 1 calc R
C14 C 0.23802(18) 0.49133(18) 0.48110(15) 0.0470(4) Uani 1 1 d .
C15 C 0.32479(19) 0.64732(18) 0.52063(15) 0.0504(4) Uani 1 1 d .
H15A H 0.3963 0.6697 0.6006 0.060 Uiso 1 1 calc R
C16 C 0.2590(2) 0.36298(19) 0.56763(17) 0.0545(4) Uani 1 1 d .
C17 C 0.1818(3) 0.1938(2) 0.5152(2) 0.0780(6) Uani 1 1 d .
H17A H 0.2090 0.1238 0.5795 0.117 Uiso 1 1 calc R
H17B H 0.2243 0.1653 0.4375 0.117 Uiso 1 1 calc R
H17C H 0.0626 0.1837 0.4950 0.117 Uiso 1 1 calc R
O1 O 0.86896(14) 1.23607(15) 0.11895(13) 0.0730(4) Uani 1 1 d .
O2 O 0.33717(17) 0.39390(15) 0.67805(13) 0.0754(4) Uani 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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C6 N1 C11 121.71(12)
C6 N1 C9 118.84(12)
C11 N1 C9 118.40(13)
O1 C2 C3 120.90(15)
O1 C2 C1 120.08(15)
C3 C2 C1 119.02(14)
C4 C3 C8 116.75(14)
C4 C3 C2 123.58(14)
C8 C3 C2 119.67(14)
C5 C4 C3 122.06(14)
C4 C5 C6 120.79(14)
N1 C6 C5 121.04(13)
N1 C6 C7 121.43(13)
C5 C6 C7 117.49(14)
C8 C7 C6 120.63(14)
C7 C8 C3 122.27(14)
C15 C10 C11 120.38(14)
C12 C11 C10 118.58(14)
C12 C11 N1 120.79(14)
C10 C11 N1 120.58(14)
C11 C12 C13 120.76(14)
C14 C13 C12 121.10(15)
C13 C14 C15 117.95(14)
C13 C14 C16 122.14(15)
C15 C14 C16 119.90(14)
C10 C15 C14 121.24(14)
O2 C16 C14 121.21(15)
O2 C16 C17 120.40(16)
C14 C16 C17 118.39(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C6 1.3954(19)
N1 C11 1.4183(19)
N1 C9 1.4561(18)
C1 C2 1.499(2)
C2 O1 1.2237(18)
C2 C3 1.481(2)
C3 C4 1.392(2)
C3 C8 1.392(2)
C4 C5 1.376(2)
C5 C6 1.398(2)
C6 C7 1.4056(19)
C7 C8 1.370(2)
C10 C15 1.374(2)
C10 C11 1.395(2)
C11 C12 1.382(2)
C12 C13 1.383(2)
C13 C14 1.383(2)
C14 C15 1.395(2)
C14 C16 1.490(2)
C16 O2 1.2154(19)
C16 C17 1.496(2)
