#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316060.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_4316060
loop_
_publ_author_name
'Subrata Naiya'
'Chaitali Biswas'
'Michael G. B. Drew'
'Carlos J. Gómez-García'
'Juan M. Clemente-Juan'
'Ashutosh Ghosh'
_publ_section_title
;
 A Unique Example of Structural and Magnetic Diversity in Four
 Interconvertible Copper(II)-Azide Complexes with the Same Schiff Base
 Ligand: A Monomer, a Dimer, a Chain, and a Layer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6616
_journal_page_last               6627
_journal_paper_doi               10.1021/ic1005456
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C12 H17 Cu N5 O'
_chemical_formula_weight         310.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.96(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.783(4)
_cell_length_b                   19.194(5)
_cell_length_c                   12.154(3)
_cell_measurement_reflns_used    18932
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.52
_cell_volume                     2738.5(14)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.3258
_diffrn_reflns_av_sigmaI/netI    0.4923
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18932
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.835
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.2663
_refine_ls_R_factor_gt           0.1043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0438P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                2048
_reflns_number_total             7928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1005456_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2738.4(13)
_cod_database_code               4316060
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
CuA Cu 0.75898(13) 0.26198(6) 0.63829(8) 0.0468(4) Uani 1 1 d . . .
N1A N 0.6933(8) 0.1740(4) 0.6807(7) 0.060(3) Uani 1 1 d . . .
N2A N 0.6498(8) 0.1639(4) 0.7671(6) 0.048(2) Uani 1 1 d . . .
N3A N 0.6052(7) 0.1532(4) 0.8454(5) 0.038(2) Uani 1 1 d . . .
O11A O 0.6774(7) 0.3146(3) 0.7400(4) 0.0493(19) Uani 1 1 d . . .
C12A C 0.6481(11) 0.3799(5) 0.7208(7) 0.049(3) Uani 1 1 d . . .
C13A C 0.5463(11) 0.3990(5) 0.7735(7) 0.054(3) Uani 1 1 d . . .
H13A H 0.5087 0.3684 0.8172 0.065 Uiso 1 1 calc R . .
C14A C 0.5098(11) 0.4681(6) 0.7526(8) 0.059(3) Uani 1 1 d . . .
H14A H 0.4522 0.4859 0.7922 0.071 Uiso 1 1 calc R . .
C15A C 0.5544(10) 0.5090(5) 0.6781(8) 0.051(3) Uani 1 1 d . . .
H15A H 0.5193 0.5510 0.6573 0.061 Uiso 1 1 calc R . .
C16A C 0.6514(12) 0.4892(5) 0.6327(7) 0.056(3) Uani 1 1 d . . .
H16A H 0.6877 0.5205 0.5890 0.067 Uiso 1 1 calc R . .
C17A C 0.6950(9) 0.4255(4) 0.6499(6) 0.034(2) Uani 1 1 d . . .
C18A C 0.8102(10) 0.4076(5) 0.6007(6) 0.044(3) Uani 1 1 d . . .
C19A C 0.8747(10) 0.4643(5) 0.5665(6) 0.050(3) Uani 1 1 d . . .
H19A H 0.9518 0.4602 0.5984 0.075 Uiso 1 1 calc R . .
H19B H 0.8425 0.5071 0.5905 0.075 Uiso 1 1 calc R . .
H19C H 0.8737 0.4642 0.4874 0.075 Uiso 1 1 calc R . .
N20A N 0.8331(7) 0.3447(4) 0.5922(5) 0.0317(18) Uani 1 1 d . . .
C21A C 0.9470(12) 0.3281(5) 0.5441(7) 0.065(4) Uani 1 1 d . . .
H21A H 1.0092 0.3243 0.6014 0.078 Uiso 1 1 calc R . .
H21B H 0.9657 0.3625 0.4901 0.078 Uiso 1 1 calc R . .
C22A C 0.9158(12) 0.2541(5) 0.4877(7) 0.056(3) Uani 1 1 d . . .
H22A H 0.8541 0.2598 0.4301 0.067 Uiso 1 1 calc R . .
H22B H 0.9814 0.2358 0.4542 0.067 Uiso 1 1 calc R . .
N23A N 0.8847(8) 0.2100(4) 0.5631(5) 0.045(2) Uani 1 1 d . . .
C25A C 0.8277(11) 0.1450(5) 0.5026(8) 0.063(3) Uani 1 1 d . . .
H25A H 0.7646 0.1599 0.4530 0.095 Uiso 1 1 calc R . .
H25B H 0.8011 0.1136 0.5562 0.095 Uiso 1 1 calc R . .
H25C H 0.8826 0.1217 0.4616 0.095 Uiso 1 1 calc R . .
C24A C 0.9736(14) 0.1884(7) 0.6473(9) 0.096(5) Uani 1 1 d . . .
H24A H 0.9396 0.1646 0.7057 0.145 Uiso 1 1 calc R . .
H24B H 1.0138 0.2287 0.6766 0.145 Uiso 1 1 calc R . .
H24C H 1.0258 0.1577 0.6150 0.145 Uiso 1 1 calc R . .
CuB Cu 0.49495(12) 0.20787(5) 0.44627(8) 0.0389(4) Uani 1 1 d . . .
N1B N 0.6111(7) 0.2797(4) 0.4770(5) 0.041(2) Uani 1 1 d . . .
N2B N 0.6496(7) 0.3144(4) 0.4021(6) 0.042(2) Uani 1 1 d . . .
N3B N 0.6902(9) 0.3393(5) 0.3325(7) 0.073(3) Uani 1 1 d . . .
O11B O 0.5797(7) 0.1678(3) 0.3337(5) 0.053(2) Uani 1 1 d . . .
C12B C 0.5697(11) 0.0977(5) 0.3198(7) 0.052(3) Uani 1 1 d . . .
C13B C 0.6725(12) 0.0800(5) 0.2573(7) 0.059(3) Uani 1 1 d . . .
H13B H 0.7233 0.1139 0.2378 0.071 Uiso 1 1 calc R . .
C14B C 0.6859(11) 0.0097(5) 0.2309(7) 0.055(3) Uani 1 1 d . . .
H14B H 0.7479 -0.0049 0.1943 0.066 Uiso 1 1 calc R . .
C15B C 0.6047(10) -0.0378(5) 0.2604(7) 0.045(3) Uani 1 1 d . . .
H15B H 0.6106 -0.0843 0.2400 0.054 Uiso 1 1 calc R . .
C16B C 0.5205(11) -0.0184(5) 0.3162(7) 0.048(3) Uani 1 1 d . . .
H16B H 0.4691 -0.0521 0.3352 0.058 Uiso 1 1 calc R . .
C17B C 0.5031(10) 0.0511(4) 0.3492(7) 0.042(3) Uani 1 1 d . . .
C18B C 0.4001(10) 0.0682(5) 0.4067(6) 0.044(3) Uani 1 1 d . . .
N20B N 0.3899(7) 0.1313(4) 0.4415(5) 0.0327(19) Uani 1 1 d . . .
C21B C 0.2915(10) 0.1483(5) 0.4963(6) 0.048(3) Uani 1 1 d . . .
H21C H 0.3005 0.1292 0.5705 0.057 Uiso 1 1 calc R . .
H21D H 0.2258 0.1260 0.4576 0.057 Uiso 1 1 calc R . .
C22B C 0.2683(13) 0.2260(5) 0.5038(7) 0.070(4) Uani 1 1 d . . .
H22C H 0.2373 0.2441 0.4329 0.084 Uiso 1 1 calc R . .
H22D H 0.2147 0.2354 0.5583 0.084 Uiso 1 1 calc R . .
N23B N 0.3787(9) 0.2576(4) 0.5367(5) 0.052(3) Uani 1 1 d . . .
C25B C 0.4214(11) 0.2446(5) 0.6548(6) 0.062(4) Uani 1 1 d . . .
H25D H 0.3650 0.2595 0.7022 0.094 Uiso 1 1 calc R . .
H25E H 0.4905 0.2703 0.6721 0.094 Uiso 1 1 calc R . .
H25F H 0.4359 0.1958 0.6656 0.094 Uiso 1 1 calc R . .
C24B C 0.3841(13) 0.3357(4) 0.5153(7) 0.065(4) Uani 1 1 d . . .
H24D H 0.3833 0.3439 0.4374 0.097 Uiso 1 1 calc R . .
H24E H 0.4528 0.3543 0.5521 0.097 Uiso 1 1 calc R . .
H24F H 0.3194 0.3580 0.5431 0.097 Uiso 1 1 calc R . .
C19B C 0.3199(9) 0.0129(4) 0.4189(7) 0.041(3) Uani 1 1 d . . .
H19D H 0.2595 0.0294 0.4602 0.061 Uiso 1 1 calc R . .
H19E H 0.3578 -0.0254 0.4574 0.061 Uiso 1 1 calc R . .
H19F H 0.2889 -0.0024 0.3473 0.061 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
O11A CuA N20A 91.0(3) . . ?
O11A CuA N1A 93.1(3) . . ?
N20A CuA N1A 175.6(3) . . ?
O11A CuA N23A 163.5(3) . . ?
N20A CuA N23A 84.8(3) . . ?
N1A CuA N23A 90.9(3) . . ?
N2A N1A CuA 124.8(6) . . ?
N3A N2A N1A 177.0(10) . . ?
C12A O11A CuA 121.8(6) . . ?
O11A C12A C17A 127.1(11) . . ?
O11A C12A C13A 112.1(10) . . ?
C17A C12A C13A 120.4(9) . . ?
C14A C13A C12A 114.1(10) . . ?
C15A C14A C13A 122.8(11) . . ?
C14A C15A C16A 120.0(10) . . ?
C17A C16A C15A 121.1(11) . . ?
C16A C17A C12A 120.7(11) . . ?
C16A C17A C18A 118.3(9) . . ?
C12A C17A C18A 120.5(9) . . ?
N20A C18A C19A 126.8(11) . . ?
N20A C18A C17A 116.4(9) . . ?
C19A C18A C17A 116.8(8) . . ?
C18A N20A C21A 115.7(9) . . ?
C18A N20A CuA 132.2(8) . . ?
C21A N20A CuA 111.9(6) . . ?
N20A C21A C22A 99.8(9) . . ?
N23A C22A C21A 109.7(7) . . ?
C22A N23A C24A 116.3(10) . . ?
C22A N23A C25A 108.5(7) . . ?
C24A N23A C25A 110.8(8) . . ?
C22A N23A CuA 104.5(6) . . ?
C24A N23A CuA 109.0(6) . . ?
C25A N23A CuA 107.3(7) . . ?
N20B CuB O11B 92.6(3) . . ?
N20B CuB N1B 169.9(3) . . ?
O11B CuB N1B 91.2(3) . . ?
N20B CuB N23B 85.1(3) . . ?
O11B CuB N23B 166.9(3) . . ?
N1B CuB N23B 93.3(3) . . ?
N2B N1B CuB 122.0(5) . . ?
N3B N2B N1B 172.6(11) . . ?
C12B O11B CuB 116.1(7) . . ?
C17B C12B O11B 135.7(11) . . ?
C17B C12B C13B 121.6(9) . . ?
O11B C12B C13B 102.7(10) . . ?
C14B C13B C12B 116.2(11) . . ?
C15B C14B C13B 118.6(11) . . ?
C16B C15B C14B 121.2(10) . . ?
C15B C16B C17B 123.6(11) . . ?
C12B C17B C16B 118.7(11) . . ?
C12B C17B C18B 121.9(8) . . ?
C16B C17B C18B 119.1(10) . . ?
N20B C18B C19B 125.3(10) . . ?
N20B C18B C17B 117.6(9) . . ?
C19B C18B C17B 117.1(8) . . ?
C18B N20B C21B 118.0(9) . . ?
C18B N20B CuB 130.5(8) . . ?
C21B N20B CuB 111.1(6) . . ?
N20B C21B C22B 114.2(10) . . ?
N23B C22B C21B 105.2(10) . . ?
C22B N23B C25B 114.3(8) . . ?
C22B N23B C24B 114.2(9) . . ?
C25B N23B C24B 108.1(7) . . ?
C22B N23B CuB 106.2(6) . . ?
C25B N23B CuB 104.5(7) . . ?
C24B N23B CuB 109.0(7) . . ?
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
CuA O11A 1.917(6) . ?
CuA N20A 1.918(8) . ?
CuA N1A 1.946(8) . ?
CuA N23A 2.064(8) . ?
N1A N2A 1.222(10) . ?
N2A N3A 1.146(9) . ?
O11A C12A 1.315(10) . ?
C12A C17A 1.376(13) . ?
C12A C13A 1.456(16) . ?
C13A C14A 1.410(13) . ?
C14A C15A 1.341(14) . ?
C15A C16A 1.367(16) . ?
C16A C17A 1.336(13) . ?
C17A C18A 1.567(15) . ?
C18A N20A 1.244(11) . ?
C18A C19A 1.410(13) . ?
N20A C21A 1.543(15) . ?
C21A C22A 1.606(13) . ?
C22A N23A 1.322(11) . ?
N23A C24A 1.459(14) . ?
N23A C25A 1.570(11) . ?
CuB N20B 1.919(8) . ?
CuB O11B 1.923(7) . ?
CuB N1B 1.957(8) . ?
CuB N23B 2.063(9) . ?
N1B N2B 1.245(10) . ?
N2B N3B 1.115(10) . ?
O11B C12B 1.359(11) . ?
C12B C17B 1.262(14) . ?
C12B C13B 1.522(17) . ?
C13B C14B 1.398(13) . ?
C14B C15B 1.392(15) . ?
C15B C16B 1.303(14) . ?
C16B C17B 1.413(12) . ?
C17B C18B 1.488(15) . ?
C18B N20B 1.292(11) . ?
C18B C19B 1.438(13) . ?
N20B C21B 1.425(13) . ?
C21B C22B 1.522(13) . ?
C22B N23B 1.459(15) . ?
N23B C25B 1.500(10) . ?
N23B C24B 1.524(11) . ?
