#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:10:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179716 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/18/7001821.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_7001821
loop_
_publ_author_name
'Chin, Aileen'
'Edgar, Mark'
'Harding, Charles J'
'McKee, Vickie'
'Nelson, Jane'
_publ_section_title
;
 A novel trisprotonated β-dialdiminate cryptand
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              6315
_journal_page_last               6326
_journal_paper_doi               10.1039/b821237f
_journal_year                    2009
_chemical_formula_sum            'C21 H45 N11 O12'
_chemical_formula_weight         643.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.4018(5)
_cell_length_b                   8.4018(5)
_cell_length_c                   26.022(2)
_cell_measurement_reflns_used    5030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      2.80
_cell_volume                     1590.80(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11497
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9913
_exptl_absorpt_correction_T_min  0.9762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Fitted as nitrate + 3 H2O
;
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0697
_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)+(0.0817P)²+3.1216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2440
_refine_ls_wR_factor_ref         0.2459
_reflns_number_gt                842
_reflns_number_total             967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821237f.txt
_cod_data_source_block           agmimsq
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1590.78(19)
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               7001821
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 1.0000 1.0000 0.0949(2) 0.0326(12) Uani 1 3 d S . .
C1 C 0.8202(5) 0.8512(5) 0.07673(15) 0.0356(10) Uani 1 1 d . . .
H1A H 0.8216 0.7365 0.0768 0.043 Uiso 1 1 calc R . .
H1B H 0.8016 0.8768 0.0416 0.043 Uiso 1 1 calc R . .
C2 C 0.6609(5) 0.8288(5) 0.10930(16) 0.0374(10) Uani 1 1 d . . .
H2A H 0.6726 0.9483 0.1150 0.045 Uiso 1 1 calc R . .
H2B H 0.5466 0.7531 0.0910 0.045 Uiso 1 1 calc R . .
N3 N 0.6548(4) 0.7440(4) 0.15882(13) 0.0384(9) Uani 1 1 d . . .
H3N H 0.6320 0.6321 0.1583 0.046 Uiso 1 1 calc R . .
C3 C 0.6807(5) 0.8217(5) 0.20373(15) 0.0361(10) Uani 1 1 d . . .
H3 H 0.7094 0.9439 0.2048 0.043 Uiso 1 1 calc R . .
C4 C 0.6682(7) 0.7345(7) 0.2500 0.0369(13) Uani 1 2 d S . .
H4 H 0.6513 0.6164 0.2500 0.044 Uiso 1 2 calc SR . .
O11 O 0.5280(4) 0.3484(4) 0.17072(14) 0.0516(10) Uani 1 1 d . . .
N11 N 0.6667 0.3333 0.1706(2) 0.0270(12) Uani 1 3 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0261(16) 0.0261(16) 0.045(3) 0.000 0.000 0.0131(8)
C1 0.0285(19) 0.0276(19) 0.050(2) -0.0011(16) -0.0012(16) 0.0133(16)
C2 0.028(2) 0.0278(19) 0.056(2) 0.0019(17) -0.0043(17) 0.0143(15)
N3 0.0337(18) 0.0204(15) 0.063(2) 0.0052(14) 0.0040(15) 0.0150(13)
C3 0.0293(19) 0.0215(18) 0.059(2) 0.0001(16) 0.0014(17) 0.0136(15)
C4 0.032(3) 0.023(2) 0.059(3) 0.000 0.000 0.016(2)
O11 0.0244(15) 0.0291(15) 0.105(3) -0.0030(15) -0.0027(15) 0.0162(12)
N11 0.0200(16) 0.0200(16) 0.041(3) 0.000 0.000 0.0100(8)
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
C1 N1 C1 110.2(2) . 2_765 ?
C1 N1 C1 110.2(2) . 3_675 ?
C1 N1 C1 110.2(2) 2_765 3_675 ?
N1 C1 C2 113.1(3) . . ?
N3 C2 C1 111.6(3) . . ?
C3 N3 C2 126.2(3) . . ?
N3 C3 C4 124.4(4) . . ?
C3 C4 C3 120.7(5) 10_556 . ?
O11 N11 O11 119.999(5) 2_655 3_665 ?
O11 N11 O11 119.999(5) 2_655 . ?
O11 N11 O11 119.999(5) 3_665 . ?
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
N1 C1 1.476(4) . ?
N1 C1 1.476(4) 2_765 ?
N1 C1 1.476(4) 3_675 ?
C1 C2 1.514(5) . ?
C2 N3 1.461(5) . ?
N3 C3 1.303(5) . ?
C3 C4 1.386(5) . ?
C4 C3 1.386(5) 10_556 ?
O11 N11 1.233(3) . ?
N11 O11 1.233(3) 2_655 ?
N11 O11 1.233(3) 3_665 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N O11 0.86 2.11 2.956(4) 166.0 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.030 0.460 0.500 166.7 62.8
2 -0.028 0.461 1.000 166.8 62.8
