#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:12:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178619 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/30/4073033.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_4073033
loop_
_publ_author_name
'Jaroschik, Florian'
'Nief, François'
'Le Goff, Xavier-Frédéric'
'Ricard, Louis'
_publ_section_title
;
 Isolation of Stable Organodysprosium(II) Complexes by Chemical Reduction
 of Dysprosium(III) Precursors
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1123
_journal_paper_doi               10.1021/om0700213
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         C28H22?
_chemical_formula_sum            'C14 H11'
_chemical_formula_weight         179.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.346(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.776(5)
_cell_length_b                   21.241(5)
_cell_length_c                   7.906(5)
_cell_measurement_reflns_used    382
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     964.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2759
_diffrn_reflns_theta_full        23.81
_diffrn_reflns_theta_max         23.81
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9972
_exptl_absorpt_correction_T_min  0.9794
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.124
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0400
_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)+(0.0423P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                1044
_reflns_number_total             1374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0700213si20070109_034632.cif
_cod_data_source_block           fj_stilbene
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P21/c     '
_cod_database_code               4073033
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C -0.1584(3) 0.12639(7) 0.51643(19) 0.0310(5) Uani 1 1 d .
H1 H -0.2745 0.1071 0.5752 0.037 Uiso 1 1 calc R
C2 C -0.1826(3) 0.18874(7) 0.4674(2) 0.0359(5) Uani 1 1 d .
H2 H -0.3135 0.2122 0.4949 0.043 Uiso 1 1 calc R
C3 C -0.0175(3) 0.21735(8) 0.3787(2) 0.0379(5) Uani 1 1 d .
H3 H -0.0350 0.2602 0.3449 0.045 Uiso 1 1 calc R
C4 C 0.1731(3) 0.18308(7) 0.3398(2) 0.0365(5) Uani 1 1 d .
H4 H 0.2863 0.2022 0.2780 0.044 Uiso 1 1 calc R
C5 C 0.1992(3) 0.12081(7) 0.39067(19) 0.0316(5) Uani 1 1 d .
H5 H 0.3312 0.0977 0.3639 0.038 Uiso 1 1 calc R
C6 C 0.0350(3) 0.09161(7) 0.48037(18) 0.0280(4) Uani 1 1 d .
C7 C 0.0733(3) 0.02533(7) 0.54257(19) 0.0280(4) Uani 1 1 d .
C8 C 0.2407(3) 0.01198(7) 0.67062(19) 0.0307(4) Uani 1 1 d .
H8 H 0.2609 -0.0315 0.6968 0.037 Uiso 1 1 calc R
C9 C 0.3967(3) 0.05502(7) 0.77564(18) 0.0277(4) Uani 1 1 d .
C10 C 0.3340(3) 0.11572(7) 0.8210(2) 0.0341(5) Uani 1 1 d .
H10 H 0.1861 0.1320 0.7778 0.041 Uiso 1 1 calc R
C11 C 0.4841(3) 0.15232(8) 0.9276(2) 0.0384(5) Uani 1 1 d .
H11 H 0.4373 0.1933 0.9577 0.046 Uiso 1 1 calc R
C12 C 0.7014(3) 0.13020(8) 0.9913(2) 0.0372(5) Uani 1 1 d .
H12 H 0.8043 0.1558 1.0639 0.045 Uiso 1 1 calc R
C13 C 0.7662(3) 0.07056(8) 0.9480(2) 0.0351(5) Uani 1 1 d .
H13 H 0.9158 0.0550 0.9898 0.042 Uiso 1 1 calc R
C14 C 0.6149(3) 0.03308(7) 0.84373(19) 0.0322(5) Uani 1 1 d .
H14 H 0.6607 -0.0085 0.8180 0.039 Uiso 1 1 calc R
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'
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
C2 C1 C6 120.58(16) . .
C2 C1 H1 119.7 . .
C6 C1 H1 119.7 . .
C1 C2 C3 120.53(16) . .
C1 C2 H2 119.7 . .
C3 C2 H2 119.7 . .
C4 C3 C2 119.44(16) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 120.11(16) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
C4 C5 C6 121.00(16) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C5 C6 C1 118.32(15) . .
C5 C6 C7 120.10(15) . .
C1 C6 C7 121.52(14) . .
C8 C7 C7 120.87(18) . 3_556
C8 C7 C6 120.70(14) . .
C7 C7 C6 118.42(17) 3_556 .
C7 C8 C9 129.39(15) . .
C7 C8 H8 115.3 . .
C9 C8 H8 115.3 . .
C14 C9 C10 117.27(14) . .
C14 C9 C8 118.70(15) . .
C10 C9 C8 123.90(16) . .
C11 C10 C9 120.90(16) . .
C11 C10 H10 119.5 . .
C9 C10 H10 119.5 . .
C10 C11 C12 120.99(16) . .
C10 C11 H11 119.5 . .
C12 C11 H11 119.5 . .
C13 C12 C11 118.95(15) . .
C13 C12 H12 120.5 . .
C11 C12 H12 120.5 . .
C12 C13 C14 120.42(17) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C13 C14 C9 121.44(16) . .
C13 C14 H14 119.3 . .
C9 C14 H14 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.383(2) .
C1 C6 1.395(2) .
C1 H1 0.9500 .
C2 C3 1.385(2) .
C2 H2 0.9500 .
C3 C4 1.382(3) .
C3 H3 0.9500 .
C4 C5 1.386(2) .
C4 H4 0.9500 .
C5 C6 1.391(2) .
C5 H5 0.9500 .
C6 C7 1.499(2) .
C7 C8 1.351(2) .
C7 C7 1.484(3) 3_556
C8 C9 1.473(2) .
C8 H8 0.9500 .
C9 C14 1.395(2) .
C9 C10 1.397(2) .
C10 C11 1.380(2) .
C10 H10 0.9500 .
C11 C12 1.382(2) .
C11 H11 0.9500 .
C12 C13 1.375(2) .
C12 H12 0.9500 .
C13 C14 1.385(2) .
C13 H13 0.9500 .
C14 H14 0.9500 .
