#------------------------------------------------------------------------------
#$Date: 2020-01-27 18:26:21 +0200 (Mon, 27 Jan 2020) $
#$Revision: 247260 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/73/4517357.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_4517357
loop_
_publ_author_name
'Anthony, S. Philip'
'Raghavaiah, P.'
'Radhakrishnan, T. P.'
_publ_section_title
;
 Extreme Molecular Orientations in a Dimorphic System: Polar/Centric and
 Polar/Polar Cogrowth Crystal Architectures
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              631
_journal_paper_doi               10.1021/cg0340594
_journal_volume                  3
_journal_year                    2003
_chemical_formula_moiety         C19H26N2O4Zn
_chemical_formula_sum            'C9.5 H13 N O2 Zn0.5'
_chemical_formula_weight         205.89
_chemical_name_systematic        Bis(acac)-(4-pyrrolidino)pyridinozinc(II)
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   11.1810(8)
_cell_length_b                   28.583(3)
_cell_length_c                   12.3090(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3933.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.259
_diffrn_measured_fraction_theta_max 0.259
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            979
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.274
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism-block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.25
_refine_diff_density_rms         0.06
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         839
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                839
_reflns_number_total             905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0340594si20030411_030205.cif
_cod_data_source_block           ZNPPA2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the built-in table derived from
the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      Fdd2(No.43)
_cod_original_formula_sum        'C9.50 H13 N O2 Zn0.50'
_cod_database_code               4517357
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.0000 0.5000 0.3699 0.0317(3) Uani 1 d S . .
N2 N 0.0000 0.5000 0.5354(5) 0.0349(14) Uani 1 d S . .
N6 N 0.0000 0.5000 0.8666(16) 0.0453(14) Uani 1 d S . .
O9 O 0.1331(3) 0.44998(10) 0.3603(4) 0.0434(8) Uani 1 d . . .
O13 O -0.1134(3) 0.45481(12) 0.3031(4) 0.0442(8) Uani 1 d . . .
C3 C 0.1029(5) 0.49854(18) 0.5942(5) 0.0429(14) Uani 1 d . . .
H3 H 0.1747 0.4975 0.5561 0.051 Uiso 1 calc R . .
C4 C 0.1088(6) 0.49850(19) 0.7070(6) 0.0500(19) Uani 1 d . . .
H4 H 0.1819 0.4975 0.7429 0.060 Uiso 1 calc R . .
C5 C 0.0000 0.5000 0.7654(7) 0.0345(17) Uani 1 d S . .
C7 C 0.1086(5) 0.49799(19) 0.9416(5) 0.0474(15) Uani 1 d . . .
H7A H 0.1600 0.4722 0.9206 0.057 Uiso 1 calc R . .
H7B H 0.1541 0.5268 0.9356 0.057 Uiso 1 calc R . .
C8 C 0.0683(6) 0.4916(3) 1.0542(7) 0.0602(18) Uani 1 d . . .
H8A H 0.1157 0.5104 1.1036 0.072 Uiso 1 calc R . .
H8B H 0.0743 0.4590 1.0756 0.072 Uiso 1 calc R . .
C10 C 0.1240(4) 0.41003(16) 0.3173(5) 0.0395(11) Uani 1 d . . .
C11 C 0.0218(5) 0.39217(19) 0.2679(5) 0.0472(12) Uani 1 d . . .
H11 H 0.0280 0.3629 0.2352 0.057 Uiso 1 calc R . .
C12 C -0.0892(5) 0.41436(16) 0.2632(5) 0.0426(11) Uani 1 d . . .
C14 C 0.2348(5) 0.3805(3) 0.3203(8) 0.0665(19) Uani 1 d . . .
H14A H 0.2973 0.3971 0.3573 0.100 Uiso 1 calc R . .
H14B H 0.2599 0.3736 0.2474 0.100 Uiso 1 calc R . .
H14C H 0.2183 0.3518 0.3581 0.100 Uiso 1 calc R . .
C15 C -0.1899(5) 0.3915(2) 0.2046(6) 0.0663(17) Uani 1 d . . .
H15A H -0.2596 0.4110 0.2087 0.099 Uiso 1 calc R . .
H15B H -0.2067 0.3617 0.2374 0.099 Uiso 1 calc R . .
H15C H -0.1682 0.3870 0.1298 0.099 Uiso 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'
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'
Zn Zn 0.2839 1.4301 '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
O13 Zn1 O13 131.1(3) . 2_565
O13 Zn1 N2 114.43(14) . .
O13 Zn1 N2 114.43(14) 2_565 .
O13 Zn1 O9 88.08(16) . 2_565
O13 Zn1 O9 89.20(15) 2_565 2_565
N2 Zn1 O9 93.29(15) . 2_565
O13 Zn1 O9 89.20(15) . .
O13 Zn1 O9 88.08(16) 2_565 .
N2 Zn1 O9 93.29(15) . .
O9 Zn1 O9 173.4(3) 2_565 .
C3 N2 C3 115.8(7) 2_565 .
C3 N2 Zn1 122.1(4) 2_565 .
C3 N2 Zn1 122.1(4) . .
C5 N6 C7 127.2(7) . 2_565
C5 N6 C7 127.2(7) . .
C7 N6 C7 105.6(13) 2_565 .
C10 O9 Zn1 126.3(3) . .
C12 O13 Zn1 127.5(3) . .
N2 C3 C4 124.8(6) . .
C3 C4 C5 117.8(6) . .
N6 C5 C4 120.5(4) . 2_565
N6 C5 C4 120.5(4) . .
C4 C5 C4 118.9(8) 2_565 .
C8 C7 N6 109.3(8) . .
C7 C8 C8 104.8(4) . 2_565
O9 C10 C11 125.5(5) . .
O9 C10 C14 115.6(5) . .
C11 C10 C14 118.9(5) . .
C10 C11 C12 125.6(5) . .
O13 C12 C11 125.5(4) . .
O13 C12 C15 114.9(4) . .
C11 C12 C15 119.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O13 1.988(3) .
Zn1 O13 1.988(3) 2_565
Zn1 N2 2.037(7) .
Zn1 O9 2.067(3) 2_565
Zn1 O9 2.067(3) .
N2 C3 1.360(7) 2_565
N2 C3 1.360(7) .
N6 C5 1.25(2) .
N6 C7 1.526(14) 2_565
N6 C7 1.526(14) .
O9 C10 1.263(6) .
O13 C12 1.285(6) .
C3 C4 1.391(10) .
C4 C5 1.413(9) .
C5 C4 1.413(9) 2_565
C7 C8 1.469(10) .
C8 C8 1.601(13) 2_565
C10 C11 1.391(7) .
C10 C14 1.500(7) .
C11 C12 1.395(7) .
C12 C15 1.489(7) .
