#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/04/4120445.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_4120445
loop_
_publ_author_name
'Liu, Guangfeng'
'Liu, Jie'
'Liu, Yang'
'Tao, Xutang'
_publ_section_title
;
 Oriented Single-Crystal-to-Single-Crystal Phase Transition with Dramatic
 Changes in the Dimensions of Crystals.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              590
_journal_page_last               593
_journal_paper_doi               10.1021/ja4102634
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C18 H12 Cu N2 O2, C12 H4 N4'
_chemical_formula_sum            'C30 H16 Cu N6 O2'
_chemical_formula_weight         556.03
_chemical_name_systematic
;
 ?
;
_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                77.3770(10)
_cell_angle_beta                 73.2790(10)
_cell_angle_gamma                77.9000(10)
_cell_formula_units_Z            1
_cell_length_a                   7.9932(9)
_cell_length_b                   8.2504(9)
_cell_length_c                   9.7490(11)
_cell_measurement_reflns_used    5054
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.21
_cell_volume                     593.40(11)
_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      175(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6522
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.9356
_exptl_absorpt_correction_T_min  0.6470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 Software Suite (Bruker,2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             283
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0326P)²+0.2415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                2405
_reflns_number_total             2448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4102634_si_002.cif
_cod_data_source_block           FormII175K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_Hall     '-P 1   '
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4120445
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
Cu1 Cu 0.0000 0.0000 0.0000 0.02191(9) Uani 1 2 d S
O1 O 0.07714(15) 0.09184(13) 0.13366(12) 0.0278(2) Uani 1 1 d .
N1 N 0.6102(2) -0.5738(2) 0.19836(19) 0.0460(4) Uani 1 1 d .
N2 N 0.6971(2) -0.2051(2) 0.42322(17) 0.0420(4) Uani 1 1 d .
N3 N 0.05803(16) -0.21642(15) 0.11927(13) 0.0224(3) Uani 1 1 d .
C1 C 0.6039(2) -0.4360(2) 0.20460(18) 0.0306(3) Uani 1 1 d .
C2 C 0.5982(2) -0.2625(2) 0.21144(17) 0.0265(3) Uani 1 1 d .
C3 C 0.5495(2) -0.13330(19) 0.10742(16) 0.0250(3) Uani 1 1 d .
C4 C 0.5501(2) 0.0401(2) 0.11440(17) 0.0271(3) Uani 1 1 d .
H4 H 0.5833 0.0648 0.1905 0.032 Uiso 1 1 calc R
C5 C 0.4970(2) -0.1661(2) -0.01199(17) 0.0272(3) Uani 1 1 d .
H5 H 0.4954 -0.2765 -0.0186 0.033 Uiso 1 1 calc R
C6 C 0.6523(2) -0.2316(2) 0.32986(18) 0.0298(3) Uani 1 1 d .
C7 C 0.11621(18) -0.19669(18) 0.23141(16) 0.0210(3) Uani 1 1 d .
C8 C 0.12370(19) -0.02634(18) 0.23698(16) 0.0222(3) Uani 1 1 d .
C9 C 0.1806(2) -0.0001(2) 0.35069(17) 0.0267(3) Uani 1 1 d .
H9 H 0.1877 0.1086 0.3581 0.032 Uiso 1 1 calc R
C10 C 0.2277(2) -0.1358(2) 0.45498(17) 0.0282(3) Uani 1 1 d .
H10 H 0.2632 -0.1142 0.5312 0.034 Uiso 1 1 calc R
C11 C 0.2231(2) -0.2996(2) 0.44814(17) 0.0285(3) Uani 1 1 d .
H11 H 0.2578 -0.3871 0.5174 0.034 Uiso 1 1 calc R
C12 C 0.1653(2) -0.33357(19) 0.33499(16) 0.0246(3) Uani 1 1 d .
C13 C 0.1518(2) -0.4951(2) 0.31563(18) 0.0313(4) Uani 1 1 d .
H13 H 0.1829 -0.5896 0.3806 0.038 Uiso 1 1 calc R
C14 C 0.0931(2) -0.5129(2) 0.2020(2) 0.0351(4) Uani 1 1 d .
H14 H 0.0839 -0.6189 0.1895 0.042 Uiso 1 1 calc R
C15 C 0.0469(2) -0.3693(2) 0.10426(18) 0.0290(3) Uani 1 1 d .
H15 H 0.0075 -0.3819 0.0268 0.035 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'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 O1 180.00(6) 2 .
O1 Cu1 N3 95.40(5) 2 .
O1 Cu1 N3 84.60(5) . .
O1 Cu1 N3 84.60(5) 2 2
O1 Cu1 N3 95.40(5) . 2
N3 Cu1 N3 180.00(9) . 2
C8 O1 Cu1 111.71(9) . .
C15 N3 C7 119.56(12) . .
C15 N3 Cu1 129.32(11) . .
C7 N3 Cu1 111.12(9) . .
N1 C1 C2 179.3(2) . .
C3 C2 C6 121.69(14) . .
C3 C2 C1 122.10(14) . .
C6 C2 C1 116.17(14) . .
C2 C3 C5 121.17(14) . .
C2 C3 C4 121.03(14) . .
C5 C3 C4 117.80(14) . .
C5 C4 C3 120.84(14) 2_655 .
C5 C4 H4 119.6 2_655 .
C3 C4 H4 119.6 . .
C4 C5 C3 121.36(14) 2_655 .
C4 C5 H5 119.3 2_655 .
C3 C5 H5 119.3 . .
N2 C6 C2 178.95(19) . .
N3 C7 C12 122.56(13) . .
N3 C7 C8 114.92(12) . .
C12 C7 C8 122.52(13) . .
O1 C8 C9 125.51(13) . .
O1 C8 C7 117.60(13) . .
C9 C8 C7 116.89(13) . .
C8 C9 C10 120.79(14) . .
C8 C9 H9 119.6 . .
C10 C9 H9 119.6 . .
C11 C10 C9 122.22(14) . .
C11 C10 H10 118.9 . .
C9 C10 H10 118.9 . .
C10 C11 C12 119.37(14) . .
C10 C11 H11 120.3 . .
C12 C11 H11 120.3 . .
C11 C12 C7 118.19(14) . .
C11 C12 C13 125.45(14) . .
C7 C12 C13 116.36(14) . .
C14 C13 C12 120.37(14) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C13 C14 C15 119.31(14) . .
C13 C14 H14 120.3 . .
C15 C14 H14 120.3 . .
N3 C15 C14 121.84(14) . .
N3 C15 H15 119.1 . .
C14 C15 H15 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9344(10) 2
Cu1 O1 1.9344(10) .
Cu1 N3 1.9522(12) .
Cu1 N3 1.9522(12) 2
O1 C8 1.3184(18) .
N1 C1 1.142(2) .
N2 C6 1.145(2) .
N3 C15 1.325(2) .
N3 C7 1.3564(19) .
C1 C2 1.438(2) .
C2 C3 1.377(2) .
C2 C6 1.430(2) .
C3 C5 1.439(2) .
C3 C4 1.448(2) .
C4 C5 1.348(2) 2_655
C4 H4 0.9300 .
C5 C4 1.348(2) 2_655
C5 H5 0.9300 .
C7 C12 1.412(2) .
C7 C8 1.433(2) .
C8 C9 1.385(2) .
C9 C10 1.405(2) .
C9 H9 0.9300 .
C10 C11 1.377(2) .
C10 H10 0.9300 .
C11 C12 1.411(2) .
C11 H11 0.9300 .
C12 C13 1.416(2) .
C13 C14 1.367(2) .
C13 H13 0.9300 .
C14 C15 1.404(2) .
C14 H14 0.9300 .
C15 H15 0.9300 .
