#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:11:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180172 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/68/7106875.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_7106875
loop_
_publ_author_name
'Ramkinkar Santra'
'Kaustuv Banerjee'
'Kumar Biradha'
_publ_section_title
;
 Weak Ag---Ag and Ag---Pi Interactions in Templating Regio Selective
 Single and Double [2+2] Reactions of
 N,N'-bis(3-(4-pyridyl)acryloyl)-hydrazine in the Solid State
;
_journal_name_full               Chem.Commun.
_journal_page_first              10740
_journal_paper_doi               10.1039/c1cc13994k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C32 H36 N8 O8'
_chemical_formula_weight         660.69
_chemical_name_common
;
r-1,t-3-bis(4-pyridyl)-c-2,t-4-bis(N-(3(4-pyridyl)acryloyl) -
hydrazinocarbonyl)cyclobutane,tetra hydrate
;
_chemical_name_systematic
;
r-1,t-3-bis(4-pyridyl)-c-2,t-4-bis(N-(3(4-pyridyl)acryloyl)
-hydrazinocarbonyl)cyclobutane,tetra hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.941(6)
_cell_angle_beta                 84.373(8)
_cell_angle_gamma                80.613(6)
_cell_formula_units_Z            1
_cell_length_a                   4.7469(9)
_cell_length_b                   9.6101(18)
_cell_length_c                   17.895(3)
_cell_measurement_reflns_used    2625
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.15
_cell_volume                     799.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker CCD APEX2'
_diffrn_measurement_method       hemisphere
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7661
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                1834
_reflns_number_total             2625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13994k.txt
_cod_data_source_block           MCB
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
N1 N 1.3753(5) 1.2442(2) -0.35826(13) 0.0291(6) Uani 1 1 d .
H1 H 1.1933 1.2633 -0.3615 0.035 Uiso 1 1 calc R
N2 N 1.4845(5) 1.1400(3) -0.30559(14) 0.0334(7) Uani 1 1 d .
H2 H 1.6554 1.0945 -0.3128 0.040 Uiso 1 1 calc R
O11 O 1.0759(5) 1.1756(3) -0.22957(14) 0.0611(8) Uani 1 1 d .
N11 N 1.6395(8) 0.6474(4) 0.04106(19) 0.0657(10) Uani 1 1 d .
C11 C 1.4240(13) 0.7419(5) 0.0543(2) 0.0850(16) Uani 1 1 d .
H11 H 1.3344 0.7432 0.1029 0.102 Uiso 1 1 calc R
C12 C 1.3169(14) 0.8418(7) 0.0008(3) 0.130(3) Uani 1 1 d .
H12 H 1.1574 0.9077 0.0141 0.156 Uiso 1 1 calc R
C13 C 1.4381(8) 0.8474(4) -0.07154(19) 0.0500(10) Uani 1 1 d .
C14 C 1.6615(11) 0.7471(5) -0.0858(2) 0.0747(15) Uani 1 1 d .
H14 H 1.7517 0.7417 -0.1343 0.090 Uiso 1 1 calc R
C15 C 1.7575(14) 0.6517(6) -0.0285(3) 0.116(2) Uani 1 1 d .
H15 H 1.9182 0.5851 -0.0398 0.139 Uiso 1 1 calc R
C16 C 1.3260(9) 0.9555(5) -0.1286(2) 0.0645(12) Uani 1 1 d .
H16 H 1.1402 1.0014 -0.1177 0.077 Uiso 1 1 calc R
C17 C 1.4538(8) 0.9950(3) -0.19238(18) 0.0385(8) Uani 1 1 d .
H17 H 1.6363 0.9488 -0.2068 0.046 Uiso 1 1 calc R
C18 C 1.3169(7) 1.1119(3) -0.24311(17) 0.0351(8) Uani 1 1 d .
O21 O 1.8098(4) 1.2919(2) -0.40376(12) 0.0374(6) Uani 1 1 d .
N21 N 0.9429(6) 1.9189(3) -0.35723(16) 0.0439(8) Uani 1 1 d .
C21 C 0.9302(8) 1.7842(4) -0.3351(2) 0.0492(9) Uani 1 1 d .
H21 H 0.7935 1.7651 -0.2963 0.059 Uiso 1 1 calc R
C22 C 1.1053(7) 1.6709(3) -0.36575(18) 0.0392(8) Uani 1 1 d .
H22 H 1.0875 1.5790 -0.3472 0.047 Uiso 1 1 calc R
C23 C 1.3084(6) 1.6952(3) -0.42454(16) 0.0279(7) Uani 1 1 d .
C24 C 1.3258(7) 1.8345(3) -0.44706(18) 0.0382(8) Uani 1 1 d .
H24 H 1.4618 1.8567 -0.4854 0.046 Uiso 1 1 calc R
C25 C 1.1412(8) 1.9413(3) -0.41278(19) 0.0401(8) Uani 1 1 d .
H25 H 1.1567 2.0344 -0.4296 0.048 Uiso 1 1 calc R
C26 C 1.5070(6) 1.5728(3) -0.45719(15) 0.0247(7) Uani 1 1 d .
H26 H 1.6813 1.5570 -0.4304 0.030 Uiso 1 1 calc R
C27 C 1.3999(6) 1.4291(3) -0.45671(15) 0.0241(7) Uani 1 1 d .
H27 H 1.1912 1.4391 -0.4467 0.029 Uiso 1 1 calc R
C28 C 1.5504(6) 1.3152(3) -0.40401(15) 0.0240(7) Uani 1 1 d .
O1W O 0.2476(8) 1.5329(4) -0.1773(2) 0.0833(12) Uani 1 1 d .
H1W2 H 0.579(9) 1.479(4) -0.223(2) 0.050 Uiso 1 1 d .
H2W2 H 0.828(9) 1.386(5) -0.248(2) 0.050 Uiso 1 1 d .
O2W O 0.7797(9) 1.4641(4) -0.2495(2) 0.0840(11) Uani 1 1 d .
H1W1 H 0.250(8) 1.486(4) -0.135(2) 0.050 Uiso 1 1 d .
H2W1 H 0.150(9) 1.514(5) -0.197(3) 0.050 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_3
C28 N1 N2 120.5(2) .
C18 N2 N1 118.3(2) .
C11 N11 C15 115.4(4) .
N11 C11 C12 123.4(4) .
C13 C12 C11 121.7(5) .
C14 C13 C12 115.0(3) .
C14 C13 C16 123.3(3) .
C12 C13 C16 121.7(4) .
C13 C14 C15 119.5(4) .
N11 C15 C14 124.9(5) .
C17 C16 C13 128.0(4) .
C16 C17 C18 121.8(3) .
O11 C18 N2 123.3(3) .
O11 C18 C17 123.4(3) .
N2 C18 C17 113.3(3) .
C25 N21 C21 115.7(3) .
N21 C21 C22 124.5(3) .
C21 C22 C23 119.4(3) .
C24 C23 C22 116.4(3) .
C24 C23 C26 123.4(3) .
C22 C23 C26 120.1(3) .
C23 C24 C25 120.1(3) .
N21 C25 C24 123.8(3) .
C23 C26 C27 118.9(2) .
C23 C26 C27 121.9(2) 2_884
C27 C26 C27 91.1(2) 2_884
C28 C27 C26 113.3(2) .
C28 C27 C26 118.2(2) 2_884
C26 C27 C26 88.9(2) 2_884
O21 C28 N1 123.4(3) .
O21 C28 C27 122.1(3) .
N1 C28 C27 114.5(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C28 1.334(3) .
N1 N2 1.386(3) .
N2 C18 1.341(4) .
O11 C18 1.219(4) .
N11 C11 1.271(5) .
N11 C15 1.314(6) .
C11 C12 1.368(6) .
C12 C13 1.364(6) .
C13 C14 1.332(5) .
C13 C16 1.464(5) .
C14 C15 1.375(6) .
C16 C17 1.296(5) .
C17 C18 1.486(4) .
O21 C28 1.215(3) .
N21 C25 1.329(4) .
N21 C21 1.329(4) .
C21 C22 1.377(5) .
C22 C23 1.386(4) .
C23 C24 1.377(4) .
C23 C26 1.505(4) .
C24 C25 1.382(4) .
C26 C27 1.546(4) .
C26 C27 1.561(4) 2_884
C27 C28 1.514(4) .
C27 C26 1.561(4) 2_884
