#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:03:07 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180166 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/62/7106220.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_7106220
loop_
_publ_author_name
'Sanjeev P. Mahanta'
'B. Sathish Kumar'
'Pradeepta K. Panda'
_publ_section_title
;
 Meso-diacylated calix[4]pyrrole: Structural diversities and enhanced
 binding towards dihydrogenphosphate ion
;
_journal_name_full               Chem.Commun.
_journal_page_first              4496
_journal_paper_doi               10.1039/c1cc10284b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C30 H36 N4 O2'
_chemical_formula_weight         484.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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            8
_cell_length_a                   21.3560(19)
_cell_length_b                   21.3560(19)
_cell_length_c                   11.329(2)
_cell_measurement_reflns_used    4162
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.70
_cell_volume                     5166.9(11)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    OLEX2
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17738
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.1076
_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)+(0.0497P)²+20.2322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                1913
_reflns_number_total             2203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10284b.txt
_cod_data_source_block           2
_cod_original_cell_volume        5167.0(12)
_cod_original_sg_symbol_H-M      'I4(1)/a '
_cod_database_code               7106220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.53628(17) 0.42261(17) 0.1281(3) 0.0379(9) Uani 1 1 d . . .
N1 N 0.41620(18) 0.52075(17) 0.1229(3) 0.0390(9) Uani 1 1 d . . .
C6 C 0.49167(18) 0.39408(18) 0.1965(3) 0.0311(9) Uani 1 1 d . . .
C4 C 0.39967(19) 0.46518(18) 0.1764(4) 0.0341(10) Uani 1 1 d . . .
C5 C 0.4414(2) 0.42968(19) 0.2613(4) 0.0378(10) Uani 1 1 d . . .
C9 C 0.5749(2) 0.37906(18) 0.0772(4) 0.0364(10) Uani 1 1 d . . .
C1 C 0.36819(19) 0.54183(19) 0.0522(4) 0.0381(10) Uani 1 1 d . . .
C3 C 0.3412(2) 0.4522(2) 0.1368(4) 0.0467(12) Uani 1 1 d . . .
H3 H 0.3177 0.4172 0.1574 0.056 Uiso 1 1 calc R . .
C2 C 0.3219(2) 0.4996(2) 0.0604(4) 0.0459(12) Uani 1 1 d . . .
H2 H 0.2836 0.5015 0.0218 0.055 Uiso 1 1 calc R . .
C11 C 0.6418(2) 0.3441(2) -0.0845(5) 0.0509(13) Uani 1 1 d . . .
O1 O 0.68690(17) 0.30919(18) -0.0824(4) 0.0730(12) Uani 1 1 d . . .
C8 C 0.5532(2) 0.32236(19) 0.1134(4) 0.0406(11) Uani 1 1 d . . .
H8 H 0.5697 0.2837 0.0921 0.049 Uiso 1 1 calc R . .
C13 C 0.4703(2) 0.4750(2) 0.3512(4) 0.0597(14) Uani 1 1 d . . .
H13A H 0.4960 0.4521 0.4055 0.090 Uiso 1 1 calc R . .
H13B H 0.4375 0.4960 0.3937 0.090 Uiso 1 1 calc R . .
H13C H 0.4954 0.5054 0.3105 0.090 Uiso 1 1 calc R . .
C7 C 0.5019(2) 0.33208(18) 0.1881(4) 0.0393(11) Uani 1 1 d . . .
H7 H 0.4789 0.3010 0.2256 0.047 Uiso 1 1 calc R . .
C10 C 0.6338(2) 0.3948(2) 0.0087(4) 0.0456(12) Uani 1 1 d . . .
C12 C 0.4003(3) 0.3824(2) 0.3292(5) 0.0633(15) Uani 1 1 d . . .
H12A H 0.3812 0.3539 0.2744 0.095 Uiso 1 1 calc R . .
H12B H 0.3683 0.4045 0.3718 0.095 Uiso 1 1 calc R . .
H12C H 0.4259 0.3593 0.3837 0.095 Uiso 1 1 calc R . .
C15 C 0.5927(2) 0.3384(2) -0.1762(5) 0.0548(13) Uani 1 1 d . . .
H15A H 0.6049 0.3618 -0.2448 0.082 Uiso 1 1 calc R . .
H15B H 0.5539 0.3545 -0.1463 0.082 Uiso 1 1 calc R . .
H15C H 0.5875 0.2951 -0.1971 0.082 Uiso 1 1 calc R . .
C14 C 0.6909(2) 0.3915(3) 0.0954(5) 0.0576(14) Uani 1 1 d . . .
H14A H 0.6870 0.4237 0.1541 0.086 Uiso 1 1 calc R . .
H14B H 0.7291 0.3974 0.0520 0.086 Uiso 1 1 calc R . .
H14C H 0.6917 0.3512 0.1332 0.086 Uiso 1 1 calc R . .
H1A H 0.450(2) 0.5383(19) 0.140(4) 0.035(12) Uiso 1 1 d . . .
H2A H 0.5425(19) 0.459(2) 0.123(4) 0.032(12) 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'
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
C9 N2 C6 110.8(3) . . ?
C1 N1 C4 110.3(4) . . ?
C7 C6 N2 106.5(4) . . ?
C7 C6 C5 130.3(4) . . ?
N2 C6 C5 123.1(3) . . ?
C3 C4 N1 105.5(4) . . ?
C3 C4 C5 130.5(4) . . ?
N1 C4 C5 124.0(4) . . ?
C6 C5 C4 111.2(3) . . ?
C6 C5 C13 110.8(4) . . ?
C4 C5 C13 110.0(4) . . ?
C6 C5 C12 108.5(3) . . ?
C4 C5 C12 108.1(4) . . ?
C13 C5 C12 108.1(4) . . ?
C8 C9 N2 105.8(4) . . ?
C8 C9 C10 129.5(4) . . ?
N2 C9 C10 124.4(4) . . ?
C2 C1 N1 106.7(4) . . ?
C2 C1 C10 127.6(4) . 9_665 ?
N1 C1 C10 125.2(4) . 9_665 ?
C4 C3 C2 109.2(4) . . ?
C1 C2 C3 108.3(4) . . ?
O1 C11 C15 121.6(5) . . ?
O1 C11 C10 120.7(5) . . ?
C15 C11 C10 117.7(4) . . ?
C9 C8 C7 108.5(4) . . ?
C6 C7 C8 108.4(4) . . ?
C9 C10 C1 114.1(3) . 9_665 ?
C9 C10 C11 106.8(4) . . ?
C1 C10 C11 108.8(4) 9_665 . ?
C9 C10 C14 108.3(4) . . ?
C1 C10 C14 110.3(4) 9_665 . ?
C11 C10 C14 108.3(4) . . ?
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
N2 C9 1.371(5) . ?
N2 C6 1.371(5) . ?
N1 C1 1.377(6) . ?
N1 C4 1.378(5) . ?
C6 C7 1.345(5) . ?
C6 C5 1.507(6) . ?
C4 C3 1.355(6) . ?
C4 C5 1.515(6) . ?
C5 C13 1.535(6) . ?
C5 C12 1.543(6) . ?
C9 C8 1.360(6) . ?
C9 C10 1.515(6) . ?
C1 C2 1.341(6) . ?
C1 C10 1.519(6) 9_665 ?
C3 C2 1.393(6) . ?
C11 O1 1.218(5) . ?
C11 C15 1.481(7) . ?
C11 C10 1.523(7) . ?
C8 C7 1.400(6) . ?
C10 C1 1.519(6) 9_665 ?
C10 C14 1.568(6) . ?
