#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/28/7012827.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_7012827
loop_
_publ_author_name
'Juan C. Mareque Rivas'
'Rafael Torres Martín de Rosales'
'Simon Parsons'
_publ_section_title
;
 Internal hydrogen bonding and amide co-ordination in zinc(II)
 complexes of a tripodal N4 ligand: structural, spectroscopic and
 reactivity studies
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2156
_journal_page_last               2163
_journal_paper_doi               10.1039/b301651j
_journal_year                    2003
_chemical_formula_moiety         'C23 H27 N5 O'
_chemical_formula_sum            'C23 H27 N5 O'
_chemical_formula_weight         389.50
_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                 90.555(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9702(9)
_cell_length_b                   9.7048(8)
_cell_length_c                   19.1103(15)
_cell_measurement_reflns_used    4680
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     2034.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       Omega
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12533
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0460
_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)+(0.0633P)²+0.5549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                4082
_reflns_number_total             4928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301651j.txt
_cod_data_source_block           rtrr92
_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.

'_exptl_absorpt_correction_type' value 'Multiscan' changed to
'multi-scan' 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_sg_symbol_H-M      P21/c
_cod_database_code               7012827
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.17541(9) 0.32294(11) 0.40633(5) 0.0201(2) Uani 1 1 d . . .
C1 C 0.21946(12) 0.46450(13) 0.39540(6) 0.0224(3) Uani 1 1 d . . .
H1A H 0.2571 0.4997 0.4392 0.027 Uiso 1 1 calc R . .
H1B H 0.1500 0.5252 0.3829 0.027 Uiso 1 1 calc R . .
C1OB C 0.19494(13) 0.57544(15) 0.01902(7) 0.0283(3) Uani 1 1 d . . .
H1OA H 0.1461 0.6179 -0.0184 0.042 Uiso 1 1 calc R . .
H1OB H 0.1421 0.5519 0.0583 0.042 Uiso 1 1 calc R . .
H1OC H 0.2337 0.4916 0.0013 0.042 Uiso 1 1 calc R . .
C1OA C 0.23501(13) 0.80963(14) 0.07030(7) 0.0264(3) Uani 1 1 d . . .
H1OD H 0.1858 0.8512 0.0328 0.040 Uiso 1 1 calc R . .
H1OE H 0.2991 0.8742 0.0849 0.040 Uiso 1 1 calc R . .
H1OF H 0.1828 0.7887 0.1102 0.040 Uiso 1 1 calc R . .
N2 N 0.27845(9) 0.52811(11) 0.27759(5) 0.0208(2) Uani 1 1 d . . .
C2 C 0.31172(11) 0.46655(13) 0.33763(6) 0.0210(3) Uani 1 1 d . . .
C3 C 0.42274(12) 0.40059(15) 0.34624(7) 0.0281(3) Uani 1 1 d . . .
H3A H 0.4436 0.3573 0.3893 0.034 Uiso 1 1 calc R . .
C4 C 0.50256(12) 0.39915(16) 0.29072(7) 0.0294(3) Uani 1 1 d . . .
H4A H 0.5795 0.3550 0.2954 0.035 Uiso 1 1 calc R . .
C5 C 0.47026(12) 0.46186(14) 0.22845(7) 0.0251(3) Uani 1 1 d . . .
H5A H 0.5241 0.4624 0.1898 0.030 Uiso 1 1 calc R . .
C6 C 0.35651(11) 0.52414(13) 0.22417(6) 0.0203(3) Uani 1 1 d . . .
N7 N 0.30912(9) 0.58439(12) 0.16302(5) 0.0224(2) Uani 1 1 d . . .
H7N H 0.2315 0.6074 0.1637 0.027 Uiso 1 1 calc R . .
O8 O 0.47849(8) 0.58760(11) 0.09570(5) 0.0302(2) Uani 1 1 d . . .
C8 C 0.37015(11) 0.61156(13) 0.10222(6) 0.0208(3) Uani 1 1 d . . .
C9 C 0.29317(11) 0.67680(13) 0.04373(6) 0.0213(3) Uani 1 1 d . . .
C10C C 0.37699(12) 0.71097(15) -0.01724(7) 0.0280(3) Uani 1 1 d . . .
H10A H 0.3292 0.7529 -0.0552 0.042 Uiso 1 1 calc R . .
H10B H 0.4154 0.6263 -0.0341 0.042 Uiso 1 1 calc R . .
H10C H 0.4401 0.7756 -0.0015 0.042 Uiso 1 1 calc R . .
C11 C 0.09998(11) 0.31472(14) 0.46890(6) 0.0226(3) Uani 1 1 d . . .
H11A H 0.0560 0.2256 0.4685 0.027 Uiso 1 1 calc R . .
H11B H 0.0382 0.3890 0.4669 0.027 Uiso 1 1 calc R . .
C12 C 0.09873(11) 0.12271(14) 0.33933(6) 0.0211(3) Uani 1 1 d . . .
N12 N -0.01165(10) 0.06561(12) 0.33047(6) 0.0243(2) Uani 1 1 d . . .
C13 C 0.20555(12) 0.04551(14) 0.33844(6) 0.0241(3) Uani 1 1 d . . .
H13A H 0.2822 0.0882 0.3469 0.029 Uiso 1 1 calc R . .
C14 C 0.19864(12) -0.09383(15) 0.32505(7) 0.0266(3) Uani 1 1 d . . .
H14A H 0.2707 -0.1479 0.3227 0.032 Uiso 1 1 calc R . .
C15 C 0.08560(13) -0.15378(15) 0.31505(7) 0.0288(3) Uani 1 1 d . . .
H15A H 0.0780 -0.2495 0.3054 0.035 Uiso 1 1 calc R . .
C16 C -0.01566(12) -0.07054(15) 0.31944(7) 0.0284(3) Uani 1 1 d . . .
H16A H -0.0935 -0.1125 0.3143 0.034 Uiso 1 1 calc R . .
C21 C 0.10422(11) 0.27695(14) 0.34542(6) 0.0225(3) Uani 1 1 d . . .
H21A H 0.1409 0.3153 0.3025 0.027 Uiso 1 1 calc R . .
H21B H 0.0203 0.3136 0.3489 0.027 Uiso 1 1 calc R . .
N22 N 0.10729(10) 0.38006(12) 0.59001(6) 0.0234(2) Uani 1 1 d . . .
C22 C 0.17026(11) 0.32701(13) 0.53678(6) 0.0201(3) Uani 1 1 d . . .
C23 C 0.28961(12) 0.28118(14) 0.54405(7) 0.0240(3) Uani 1 1 d . . .
H23A H 0.3323 0.2455 0.5050 0.029 Uiso 1 1 calc R . .
C24 C 0.34499(12) 0.28845(16) 0.60914(7) 0.0289(3) Uani 1 1 d . . .
H24A H 0.4264 0.2574 0.6156 0.035 Uiso 1 1 calc R . .
C25 C 0.28060(13) 0.34143(15) 0.66476(7) 0.0278(3) Uani 1 1 d . . .
H25A H 0.3162 0.3467 0.7102 0.033 Uiso 1 1 calc R . .
C26 C 0.16298(12) 0.38645(14) 0.65241(7) 0.0258(3) Uani 1 1 d . . .
H26A H 0.1191 0.4242 0.6905 0.031 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'
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
C11 N1 C21 109.36(9) . . ?
C11 N1 C1 110.85(10) . . ?
C21 N1 C1 110.17(10) . . ?
N1 C1 C2 109.90(10) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C9 C1OB H1OA 109.5 . . ?
C9 C1OB H1OB 109.5 . . ?
H1OA C1OB H1OB 109.5 . . ?
C9 C1OB H1OC 109.5 . . ?
H1OA C1OB H1OC 109.5 . . ?
H1OB C1OB H1OC 109.5 . . ?
C9 C1OA H1OD 109.5 . . ?
C9 C1OA H1OE 109.5 . . ?
H1OD C1OA H1OE 109.5 . . ?
C9 C1OA H1OF 109.5 . . ?
H1OD C1OA H1OF 109.5 . . ?
H1OE C1OA H1OF 109.5 . . ?
C6 N2 C2 117.94(11) . . ?
N2 C2 C3 122.65(11) . . ?
N2 C2 C1 117.00(11) . . ?
C3 C2 C1 120.25(11) . . ?
C4 C3 C2 118.46(12) . . ?
C4 C3 H3A 120.8 . . ?
C2 C3 H3A 120.8 . . ?
C5 C4 C3 119.88(12) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C4 C5 C6 117.78(12) . . ?
C4 C5 H5A 121.1 . . ?
C6 C5 H5A 121.1 . . ?
N2 C6 C5 123.27(11) . . ?
N2 C6 N7 112.87(11) . . ?
C5 C6 N7 123.81(11) . . ?
C8 N7 C6 127.29(10) . . ?
C8 N7 H7N 116.4 . . ?
C6 N7 H7N 116.4 . . ?
O8 C8 N7 122.30(12) . . ?
O8 C8 C9 122.39(11) . . ?
N7 C8 C9 115.30(10) . . ?
C1OA C9 C10C 109.08(11) . . ?
C1OA C9 C1OB 110.48(11) . . ?
C10C C9 C1OB 109.36(11) . . ?
C1OA C9 C8 109.60(10) . . ?
C10C C9 C8 108.34(10) . . ?
C1OB C9 C8 109.95(11) . . ?
C9 C10C H10A 109.5 . . ?
C9 C10C H10B 109.5 . . ?
H10A C10C H10B 109.5 . . ?
C9 C10C H10C 109.5 . . ?
H10A C10C H10C 109.5 . . ?
H10B C10C H10C 109.5 . . ?
N1 C11 C22 114.24(10) . . ?
N1 C11 H11A 108.7 . . ?
C22 C11 H11A 108.7 . . ?
N1 C11 H11B 108.7 . . ?
C22 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N12 C12 C13 122.39(12) . . ?
N12 C12 C21 117.19(11) . . ?
C13 C12 C21 120.29(11) . . ?
C16 N12 C12 117.13(12) . . ?
C14 C13 C12 119.07(12) . . ?
C14 C13 H13A 120.5 . . ?
C12 C13 H13A 120.5 . . ?
C13 C14 C15 119.12(13) . . ?
C13 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
C16 C15 C14 117.92(13) . . ?
C16 C15 H15A 121.0 . . ?
C14 C15 H15A 121.0 . . ?
N12 C16 C15 124.30(13) . . ?
N12 C16 H16A 117.9 . . ?
C15 C16 H16A 117.9 . . ?
N1 C21 C12 112.69(10) . . ?
N1 C21 H21A 109.1 . . ?
C12 C21 H21A 109.1 . . ?
N1 C21 H21B 109.1 . . ?
C12 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C26 N22 C22 117.48(11) . . ?
N22 C22 C23 122.71(11) . . ?
N22 C22 C11 114.91(11) . . ?
C23 C22 C11 122.32(11) . . ?
C24 C23 C22 118.68(12) . . ?
C24 C23 H23A 120.7 . . ?
C22 C23 H23A 120.7 . . ?
C23 C24 C25 119.24(13) . . ?
C23 C24 H24A 120.4 . . ?
C25 C24 H24A 120.4 . . ?
C26 C25 C24 118.07(12) . . ?
C26 C25 H25A 121.0 . . ?
C24 C25 H25A 121.0 . . ?
N22 C26 C25 123.81(12) . . ?
N22 C26 H26A 118.1 . . ?
C25 C26 H26A 118.1 . . ?
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 C11 1.4630(15) . ?
N1 C21 1.4651(15) . ?
N1 C1 1.4719(16) . ?
C1 C2 1.5051(17) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1OB C9 1.5304(19) . ?
C1OB H1OA 0.9800 . ?
C1OB H1OB 0.9800 . ?
C1OB H1OC 0.9800 . ?
C1OA C9 1.5275(18) . ?
C1OA H1OD 0.9800 . ?
C1OA H1OE 0.9800 . ?
C1OA H1OF 0.9800 . ?
N2 C6 1.3392(16) . ?
N2 C2 1.3411(16) . ?
C2 C3 1.3842(19) . ?
C3 C4 1.3823(19) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3798(19) . ?
C4 H4A 0.9500 . ?
C5 C6 1.3883(18) . ?
C5 H5A 0.9500 . ?
C6 N7 1.4021(16) . ?
N7 C8 1.3722(16) . ?
N7 H7N 0.8800 . ?
O8 C8 1.2185(15) . ?
C8 C9 1.5315(17) . ?
C9 C10C 1.5276(17) . ?
C10C H10A 0.9800 . ?
C10C H10B 0.9800 . ?
C10C H10C 0.9800 . ?
C11 C22 1.5073(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N12 1.3409(16) . ?
C12 C13 1.3911(18) . ?
C12 C21 1.5025(18) . ?
N12 C16 1.3388(18) . ?
C13 C14 1.378(2) . ?
C13 H13A 0.9500 . ?
C14 C15 1.3814(19) . ?
C14 H14A 0.9500 . ?
C15 C16 1.377(2) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
N22 C26 1.3361(17) . ?
N22 C22 1.3381(16) . ?
C22 C23 1.3886(18) . ?
C23 C24 1.3808(18) . ?
C23 H23A 0.9500 . ?
C24 C25 1.3812(19) . ?
C24 H24A 0.9500 . ?
C25 C26 1.380(2) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21146225
