#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:30:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179634 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/98/4509872.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_4509872
loop_
_publ_author_name
'Zhang, Rui'
'Zhao, Yanxia'
'Wang, Jiamin'
'Ji, Liguo'
'Yang, Xiao-Juan'
'Wu, Biao'
_publ_section_title
;
 Chloride Encapsulation by a Tripodal Tris(4-pyridylurea) Ligand and
 Effects of Countercations on the Secondary Coordination Sphere
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              544
_journal_paper_doi               10.1021/cg401345z
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C48 H72 Ca Cl2 N20 O12'
_chemical_formula_weight         1232.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            3
_cell_length_a                   13.241(2)
_cell_length_b                   13.241(2)
_cell_length_c                   31.070(5)
_cell_measurement_reflns_used    2431
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.02
_cell_measurement_theta_min      3.08
_cell_volume                     4717.5(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7847
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.9388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1950
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0326
_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)+(0.0300P)²+7.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                1497
_reflns_number_total             1869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401345z_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4717.7(13)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4509872
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ca1 Ca 1.0000 1.0000 0.0000 0.0338(2) Uani 1 6 d S
Cl1 Cl 0.3333 0.6667 0.11092(3) 0.0424(2) Uani 1 3 d S
O1 O 0.35277(13) 1.02559(12) 0.05016(5) 0.0486(4) Uani 1 1 d .
O2 O 0.89752(16) 0.84109(15) 0.04551(5) 0.0566(5) Uani 1 1 d .
N1 N 0.3333 0.6667 -0.01570(8) 0.0377(6) Uani 1 3 d S
N2 N 0.33891(18) 0.85023(16) 0.03938(6) 0.0554(5) Uani 1 1 d .
H2 H 0.3475 0.7961 0.0511 0.067 Uiso 1 1 calc R
N3 N 0.39491(17) 0.93668(15) 0.10483(6) 0.0502(5) Uani 1 1 d .
H3 H 0.3999 0.8758 0.1107 0.060 Uiso 1 1 calc R
N4 N 0.48061(19) 1.1645(2) 0.20958(7) 0.0661(6) Uani 1 1 d .
C1 C 0.3609(2) 0.78309(18) -0.03077(6) 0.0457(5) Uani 1 1 d .
H1A H 0.3377 0.7776 -0.0607 0.055 Uiso 1 1 calc R
H1B H 0.4446 0.8349 -0.0293 0.055 Uiso 1 1 calc R
C2 C 0.3017(2) 0.8355(2) -0.00514(7) 0.0536(6) Uani 1 1 d .
H2A H 0.3209 0.9105 -0.0173 0.064 Uiso 1 1 calc R
H2B H 0.2178 0.7849 -0.0067 0.064 Uiso 1 1 calc R
C3 C 0.36080(17) 0.94289(17) 0.06339(6) 0.0398(5) Uani 1 1 d .
C4 C 0.42230(18) 1.01577(19) 0.13837(7) 0.0450(5) Uani 1 1 d .
C5 C 0.4295(2) 0.9790(2) 0.17956(7) 0.0609(7) Uani 1 1 d .
H5 H 0.4151 0.9035 0.1842 0.073 Uiso 1 1 calc R
C6 C 0.4582(3) 1.0552(3) 0.21330(8) 0.0722(8) Uani 1 1 d .
H6 H 0.4623 1.0287 0.2406 0.087 Uiso 1 1 calc R
C7 C 0.4736(2) 1.1982(2) 0.17007(8) 0.0606(6) Uani 1 1 d .
H7 H 0.4891 1.2744 0.1665 0.073 Uiso 1 1 calc R
C8 C 0.4451(2) 1.12923(19) 0.13385(7) 0.0515(6) Uani 1 1 d .
H8 H 0.4412 1.1582 0.1070 0.062 Uiso 1 1 calc R
H2' H 0.832(3) 0.782(3) 0.0431(10) 0.086(10) Uiso 1 1 d .
H2'' H 0.922(3) 0.834(3) 0.0729(10) 0.100(10) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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
O2 Ca1 O2 180.00(7) 11_565 2_765
O2 Ca1 O2 86.91(7) 11_565 12_655
O2 Ca1 O2 93.09(7) 2_765 12_655
O2 Ca1 O2 93.09(7) 11_565 3_675
O2 Ca1 O2 86.91(7) 2_765 3_675
O2 Ca1 O2 180.00(7) 12_655 3_675
O2 Ca1 O2 86.91(7) 11_565 10_775
O2 Ca1 O2 93.09(7) 2_765 10_775
O2 Ca1 O2 86.91(7) 12_655 10_775
O2 Ca1 O2 93.09(7) 3_675 10_775
O2 Ca1 O2 93.09(7) 11_565 .
O2 Ca1 O2 86.91(7) 2_765 .
O2 Ca1 O2 93.09(7) 12_655 .
O2 Ca1 O2 86.91(7) 3_675 .
O2 Ca1 O2 180.0 10_775 .
Ca1 O2 H2' 131(2) . .
Ca1 O2 H2'' 124.8(19) . .
H2' O2 H2'' 104(3) . .
C1 N1 C1 110.39(12) . 2_665
C1 N1 C1 110.39(12) . 3_565
C1 N1 C1 110.38(12) 2_665 3_565
C3 N2 C2 123.98(18) . .
C3 N2 H2 118.0 . .
C2 N2 H2 118.0 . .
C3 N3 C4 128.60(18) . .
C3 N3 H3 115.7 . .
C4 N3 H3 115.7 . .
C7 N4 C6 115.6(2) . .
N1 C1 C2 113.62(18) . .
N1 C1 H1A 108.8 . .
C2 C1 H1A 108.8 . .
N1 C1 H1B 108.8 . .
C2 C1 H1B 108.8 . .
H1A C1 H1B 107.7 . .
N2 C2 C1 110.22(18) . .
N2 C2 H2A 109.6 . .
C1 C2 H2A 109.6 . .
N2 C2 H2B 109.6 . .
C1 C2 H2B 109.6 . .
H2A C2 H2B 108.1 . .
O1 C3 N2 123.90(19) . .
O1 C3 N3 122.97(19) . .
N2 C3 N3 113.13(18) . .
C8 C4 C5 117.3(2) . .
C8 C4 N3 125.1(2) . .
C5 C4 N3 117.6(2) . .
C6 C5 C4 119.2(2) . .
C6 C5 H5 120.4 . .
C4 C5 H5 120.4 . .
N4 C6 C5 124.4(2) . .
N4 C6 H6 117.8 . .
C5 C6 H6 117.8 . .
N4 C7 C8 125.1(2) . .
N4 C7 H7 117.4 . .
C8 C7 H7 117.4 . .
C7 C8 C4 118.4(2) . .
C7 C8 H8 120.8 . .
C4 C8 H8 120.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2 2.3264(16) 11_565
Ca1 O2 2.3264(16) 2_765
Ca1 O2 2.3264(16) 12_655
Ca1 O2 2.3264(16) 3_675
Ca1 O2 2.3264(16) 10_775
Ca1 O2 2.3265(16) .
O1 C3 1.223(2) .
O2 H2' 0.83(3) .
O2 H2'' 0.94(3) .
N1 C1 1.472(2) .
N1 C1 1.472(2) 2_665
N1 C1 1.472(2) 3_565
N2 C3 1.338(3) .
N2 C2 1.449(3) .
N2 H2 0.8600 .
N3 C3 1.381(3) .
N3 C4 1.391(3) .
N3 H3 0.8600 .
N4 C7 1.325(3) .
N4 C6 1.329(4) .
C1 C2 1.508(3) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C4 C8 1.384(3) .
C4 C5 1.389(3) .
C5 C6 1.371(3) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.378(3) .
C7 H7 0.9300 .
C8 H8 0.9300 .
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
O2 H2'' N4 0.94(3) 1.85(3) 2.778(3) 173(3) 15_655
O2 H2' O1 0.83(3) 1.98(3) 2.797(2) 168(3) 3_565
N3 H3 Cl1 0.86 2.45 3.2509(18) 155.0 .
N2 H2 Cl1 0.86 2.47 3.2673(19) 154.2 .
