#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:14:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179052 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/14/4301433.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_4301433
loop_
_publ_author_name
'Wen-Xiu Ni'
'Mian Li'
'Shun-Ze Zhan'
'Jin-Zhang Hou'
'Dan Li'
_publ_section_title
;
In Situ Immobilization of Metalloligands: A Synthetic Route to Homometallic
Mixed-Valence Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1433
_journal_page_last               1441
_journal_paper_doi               10.1021/ic8015244
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C14 H10 Cu2 N6 O'
_chemical_formula_weight         405.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 103.28
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5040(14)
_cell_length_b                   9.059(2)
_cell_length_c                   14.156(3)
_cell_measurement_reflns_used    1482
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9
_cell_measurement_theta_min      2.7
_cell_volume                     811.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX area-dectector diffractometer'
_diffrn_measurement_method       'φ and ω-scan'
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5098
_diffrn_reflns_theta_full        27.82
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0454
_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)+(0.0608P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                2538
_reflns_number_total             3070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8015244_si_002_5.cif
_cod_data_source_block           complex5
_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 'Multi-scan' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' 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 c'
_cod_database_code               4301433
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, 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
C1 C 0.7278(10) 0.8033(8) 0.0282(4) 0.0499(17) Uani 1 1 d . . .
H1 H 0.8047 0.8587 0.0797 0.060 Uiso 1 1 calc R . .
C2 C 0.8020(10) 0.7808(9) -0.0556(4) 0.0530(17) Uani 1 1 d . . .
H2 H 0.9315 0.8222 -0.0579 0.064 Uiso 1 1 calc R . .
C3 C 0.5169(11) 0.6465(7) -0.1253(4) 0.0442(14) Uani 1 1 d . . .
H3 H 0.4428 0.5914 -0.1776 0.053 Uiso 1 1 calc R . .
C4 C 0.4281(10) 0.6626(7) -0.0457(4) 0.0466(15) Uani 1 1 d . . .
H4 H 0.2975 0.6213 -0.0451 0.056 Uiso 1 1 calc R . .
C5 C 0.5396(9) 0.7419(7) 0.0324(3) 0.0383(13) Uani 1 1 d . . .
C6 C 0.4406(9) 0.7635(7) 0.1182(4) 0.0365(12) Uani 1 1 d . A .
C7 C 0.6162(11) 0.7588(9) 0.3681(4) 0.0477(18) Uani 1 1 d . . .
H7 H 0.7544 0.7295 0.3705 0.057 Uiso 1 1 calc R . .
C8 C 0.5449(9) 0.7754(8) 0.4592(4) 0.0436(14) Uani 1 1 d . . .
C9 C 0.3651(13) 0.8520(9) 0.4658(5) 0.057(2) Uani 1 1 d . . .
H9 H 0.2822 0.8976 0.4114 0.068 Uiso 1 1 calc R . .
C10 C 0.3103(11) 0.8598(8) 0.5540(4) 0.0591(19) Uani 1 1 d . . .
H10 H 0.1904 0.9110 0.5607 0.071 Uiso 1 1 calc R . .
C11 C 0.4375(12) 0.7899(9) 0.6317(5) 0.0535(19) Uani 1 1 d . . .
H11 H 0.3969 0.7916 0.6905 0.064 Uiso 1 1 calc R . .
C12 C 0.6627(12) 0.7130(8) 0.5426(5) 0.0462(16) Uani 1 1 d . . .
H12 H 0.7847 0.6622 0.5387 0.055 Uiso 1 1 calc R . .
C13 C 0.0459(10) 0.6388(6) 0.2569(5) 0.0324(14) Uani 1 1 d . A 1
C14 C 0.0565(10) 1.0171(5) 0.2479(4) 0.0293(13) Uani 1 1 d . . 1
Cu1 Cu 0.15571(8) 0.82560(7) 0.24331(4) 0.0390(2) Uani 1 1 d . . .
Cu2 Cu -0.14559(7) 0.32854(8) 0.25500(4) 0.0375(2) Uani 1 1 d . . .
N1 N 0.7011(9) 0.7046(6) -0.1318(3) 0.0383(13) Uani 1 1 d . . .
N2 N 0.5737(7) 0.7627(6) 0.2058(3) 0.0451(13) Uani 1 1 d . . .
H5 H 0.7070 0.7494 0.2117 0.054 Uiso 1 1 calc R A .
N3 N 0.4913(7) 0.7839(5) 0.2858(3) 0.0348(10) Uani 1 1 d . A .
N4 N 0.6136(9) 0.7205(6) 0.6285(3) 0.0453(12) Uani 1 1 d . . .
N5 N -0.0182(11) 0.5253(10) 0.2570(5) 0.075(2) Uani 1 1 d . A 1
N6 N 0.0025(10) 1.1349(7) 0.2543(4) 0.0474(15) Uani 1 1 d . . 1
O1 O 0.2526(7) 0.7836(6) 0.1050(3) 0.0466(11) Uani 1 1 d . A .
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
_geom_angle_publ_flag
C5 C1 C2 117.9(5) . . ?
N1 C2 C1 124.5(6) . . ?
N1 C3 C4 124.3(6) . . ?
C5 C4 C3 117.8(6) . . ?
C1 C5 C4 119.6(5) . . ?
C1 C5 C6 122.4(5) . . ?
C4 C5 C6 118.0(6) . . ?
O1 C6 N2 124.0(5) . . ?
O1 C6 C5 119.9(5) . . ?
N2 C6 C5 116.1(5) . . ?
N3 C7 C8 121.1(6) . . ?
C12 C8 C9 117.6(5) . . ?
C12 C8 C7 119.0(6) . . ?
C9 C8 C7 123.5(5) . . ?
C10 C9 C8 119.2(6) . . ?
C11 C10 C9 118.0(6) . . ?
N4 C11 C10 124.2(6) . . ?
N4 C12 C8 124.2(6) . . ?
N5 C13 Cu1 174.0(7) . . ?
N6 C14 Cu1 177.0(6) . . ?
C14 Cu1 C13 134.4(3) . . ?
C14 Cu1 N3 119.4(2) . . ?
C13 Cu1 N3 101.5(2) . . ?
C14 Cu1 O1 111.2(2) . . ?
C13 Cu1 O1 97.4(3) . . ?
N3 Cu1 O1 75.08(16) . . ?
N5 Cu2 N6 126.4(3) . 1_545 ?
N5 Cu2 N1 113.1(3) . 2_465 ?
N6 Cu2 N1 101.1(2) 1_545 2_465 ?
N5 Cu2 N4 115.2(2) . 2_464 ?
N6 Cu2 N4 94.3(2) 1_545 2_464 ?
N1 Cu2 N4 103.0(2) 2_465 2_464 ?
C2 N1 C3 115.9(5) . . ?
C2 N1 Cu2 117.7(4) . 2_664 ?
C3 N1 Cu2 126.2(4) . 2_664 ?
C6 N2 N3 118.1(4) . . ?
C7 N3 N2 116.1(5) . . ?
C7 N3 Cu1 132.5(4) . . ?
N2 N3 Cu1 110.8(3) . . ?
C11 N4 C12 116.8(5) . . ?
C11 N4 Cu2 123.1(4) . 2_665 ?
C12 N4 Cu2 118.2(4) . 2_665 ?
C13 N5 Cu2 177.2(7) . . ?
C14 N6 Cu2 169.6(6) . 1_565 ?
C6 O1 Cu1 111.8(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
C1 C5 1.358(8) . ?
C1 C2 1.395(8) . ?
C2 N1 1.322(8) . ?
C3 N1 1.331(8) . ?
C3 C4 1.387(8) . ?
C4 C5 1.376(9) . ?
C5 C6 1.512(7) . ?
C6 O1 1.208(7) . ?
C6 N2 1.339(7) . ?
C7 N3 1.278(7) . ?
C7 C8 1.476(8) . ?
C8 C12 1.373(9) . ?
C8 C9 1.381(9) . ?
C9 C10 1.377(8) . ?
C10 C11 1.370(10) . ?
C11 N4 1.317(9) . ?
C12 N4 1.328(8) . ?
C13 N5 1.110(9) . ?
C13 Cu1 1.864(5) . ?
C14 N6 1.134(7) . ?
C14 Cu1 1.857(5) . ?
Cu1 N3 2.160(4) . ?
Cu1 O1 2.223(4) . ?
Cu2 N5 1.963(9) . ?
Cu2 N6 2.003(6) 1_545 ?
Cu2 N1 2.094(5) 2_465 ?
Cu2 N4 2.138(5) 2_464 ?
N1 Cu2 2.094(5) 2_664 ?
N2 N3 1.373(6) . ?
N4 Cu2 2.138(5) 2_665 ?
N6 Cu2 2.003(6) 1_565 ?
