#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:14:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179052 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/14/4301429.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_4301429
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            'C24 H18 Cu N8 O2'
_chemical_formula_weight         514.00
_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                 105.126(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3050(11)
_cell_length_b                   9.7196(9)
_cell_length_c                   19.4917(16)
_cell_measurement_reflns_used    3949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.2
_cell_volume                     2250.4(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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13694
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0371
_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)+(0.0568P)²+0.2912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                4197
_reflns_number_total             5158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8015244_si_002_1.cif
_cod_data_source_block           complex2
_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 21/c'
_cod_database_code               4301429
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
C1 C 0.88014(18) 0.8298(2) 0.20846(12) 0.0419(5) Uani 1 1 d . . .
H1 H 0.8793 0.7710 0.2460 0.050 Uiso 1 1 calc R . .
C2 C 0.96785(18) 0.9211(3) 0.21325(13) 0.0487(6) Uani 1 1 d . . .
H2 H 1.0248 0.9223 0.2554 0.058 Uiso 1 1 calc R . .
C3 C 0.89347(19) 1.0027(2) 0.10279(13) 0.0489(6) Uani 1 1 d . . .
H3 H 0.8976 1.0608 0.0657 0.059 Uiso 1 1 calc R . .
C4 C 0.80115(19) 0.9170(2) 0.09281(12) 0.0401(5) Uani 1 1 d . . .
H4 H 0.7448 0.9193 0.0504 0.048 Uiso 1 1 calc R . .
C5 C 0.79326(16) 0.8275(2) 0.14657(11) 0.0324(4) Uani 1 1 d . . .
C6 C 0.69280(16) 0.7359(2) 0.13650(10) 0.0299(4) Uani 1 1 d . . .
C7 C 0.56783(16) 0.48566(19) 0.21194(10) 0.0290(4) Uani 1 1 d . . .
H7 H 0.4993 0.4413 0.1943 0.035 Uiso 1 1 calc R . .
C8 C 0.62965(15) 0.44086(19) 0.28275(9) 0.0276(4) Uani 1 1 d . . .
C9 C 0.57469(16) 0.34376(19) 0.31419(10) 0.0296(4) Uani 1 1 d . . .
H9 H 0.5036 0.3148 0.2886 0.036 Uiso 1 1 calc R . .
C10 C 0.72068(18) 0.3313(2) 0.41393(11) 0.0395(5) Uani 1 1 d . . .
H10 H 0.7523 0.2946 0.4588 0.047 Uiso 1 1 calc R . .
C11 C 0.78235(18) 0.4257(2) 0.38727(11) 0.0419(5) Uani 1 1 d . . .
H11 H 0.8540 0.4508 0.4136 0.050 Uiso 1 1 calc R . .
C12 C 0.73719(17) 0.4829(2) 0.32115(11) 0.0370(5) Uani 1 1 d . . .
H12 H 0.7772 0.5479 0.3025 0.044 Uiso 1 1 calc R . .
C13 C 0.10366(18) 0.4182(2) -0.05238(11) 0.0411(5) Uani 1 1 d . . .
H13 H 0.1069 0.4716 -0.0914 0.049 Uiso 1 1 calc R . .
C14 C 0.0097(2) 0.3403(3) -0.05367(14) 0.0493(6) Uani 1 1 d . . .
H14 H -0.0493 0.3427 -0.0947 0.059 Uiso 1 1 calc R . .
C15 C 0.0835(2) 0.2611(2) 0.05752(13) 0.0486(6) Uani 1 1 d . . .
H15 H 0.0770 0.2081 0.0959 0.058 Uiso 1 1 calc R . .
C16 C 0.18201(19) 0.3343(2) 0.06420(12) 0.0414(5) Uani 1 1 d . . .
H16 H 0.2398 0.3290 0.1058 0.050 Uiso 1 1 calc R . .
C17 C 0.19352(16) 0.4158(2) 0.00800(10) 0.0317(4) Uani 1 1 d . . .
C18 C 0.29708(16) 0.49921(19) 0.01516(10) 0.0300(4) Uani 1 1 d . . .
C19 C 0.42269(17) 0.7449(2) -0.06290(10) 0.0331(4) Uani 1 1 d . . .
H24 H 0.4923 0.7876 -0.0463 0.040 Uiso 1 1 calc R . .
C20 C 0.35867(17) 0.7920(2) -0.13265(10) 0.0321(4) Uani 1 1 d . . .
C21 C 0.4097(2) 0.8922(2) -0.16402(12) 0.0435(5) Uani 1 1 d . . .
H25 H 0.4809 0.9216 -0.1390 0.052 Uiso 1 1 calc R . .
C22 C 0.2640(2) 0.9068(2) -0.26121(12) 0.0465(6) Uani 1 1 d . . .
H26 H 0.2309 0.9450 -0.3055 0.056 Uiso 1 1 calc R . .
C23 C 0.2044(2) 0.8091(2) -0.23550(11) 0.0456(5) Uani 1 1 d . . .
H27 H 0.1329 0.7832 -0.2618 0.055 Uiso 1 1 calc R . .
C24 C 0.25161(18) 0.7494(2) -0.17017(11) 0.0395(5) Uani 1 1 d . . .
H28 H 0.2129 0.6827 -0.1518 0.047 Uiso 1 1 calc R . .
Cu1 Cu 0.489512(19) 0.62744(2) 0.078332(11) 0.02878(9) Uani 1 1 d . . .
N1 N 0.97672(15) 1.0075(2) 0.16193(12) 0.0507(5) Uani 1 1 d . . .
N2 N 0.69147(14) 0.64922(17) 0.18864(9) 0.0314(4) Uani 1 1 d . . .
N3 N 0.59092(13) 0.57523(17) 0.16952(8) 0.0285(3) Uani 1 1 d . . .
N4 N 0.61722(13) 0.28934(17) 0.37861(8) 0.0324(4) Uani 1 1 d . . .
N5 N -0.00240(17) 0.2617(2) -0.00021(11) 0.0496(5) Uani 1 1 d . . .
N6 N 0.29997(14) 0.58239(17) -0.03813(8) 0.0310(4) Uani 1 1 d . . .
N7 N 0.40057(14) 0.65516(17) -0.02005(8) 0.0303(4) Uani 1 1 d . . .
N8 N 0.36530(17) 0.9498(2) -0.22701(10) 0.0502(5) Uani 1 1 d . . .
O1 O 0.61534(11) 0.74880(15) 0.07849(7) 0.0361(3) Uani 1 1 d . . .
O2 O 0.37428(11) 0.48704(14) 0.07339(7) 0.0360(3) Uani 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'
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
C2 C1 C5 118.7(2) . . ?
N1 C2 C1 124.7(2) . . ?
N1 C3 C4 124.3(2) . . ?
C3 C4 C5 119.3(2) . . ?
C4 C5 C1 117.23(19) . . ?
C4 C5 C6 119.59(18) . . ?
C1 C5 C6 123.17(19) . . ?
O1 C6 N2 125.77(18) . . ?
O1 C6 C5 117.23(17) . . ?
N2 C6 C5 117.00(17) . . ?
N3 C7 C8 131.64(18) . . ?
C9 C8 C12 117.54(17) . . ?
C9 C8 C7 115.20(17) . . ?
C12 C8 C7 127.26(17) . . ?
N4 C9 C8 124.43(18) . . ?
N4 C10 C11 123.46(19) . . ?
C10 C11 C12 119.60(19) . . ?
C11 C12 C8 118.37(19) . . ?
C14 C13 C17 119.0(2) . . ?
N5 C14 C13 124.5(2) . . ?
N5 C15 C16 124.2(2) . . ?
C15 C16 C17 119.1(2) . . ?
C13 C17 C16 117.07(19) . . ?
C13 C17 C18 122.98(18) . . ?
C16 C17 C18 119.91(17) . . ?
O2 C18 N6 125.86(17) . . ?
O2 C18 C17 116.90(17) . . ?
N6 C18 C17 117.21(17) . . ?
N7 C19 C20 131.72(19) . . ?
C21 C20 C24 116.92(19) . . ?
C21 C20 C19 115.88(19) . . ?
C24 C20 C19 127.18(18) . . ?
N8 C21 C20 125.4(2) . . ?
N8 C22 C23 124.0(2) . . ?
C22 C23 C24 119.4(2) . . ?
C23 C24 C20 118.2(2) . . ?
O1 Cu1 O2 172.43(6) . . ?
O1 Cu1 N3 80.61(6) . . ?
O2 Cu1 N3 98.43(6) . . ?
O1 Cu1 N7 99.14(6) . . ?
O2 Cu1 N7 80.51(6) . . ?
N3 Cu1 N7 170.24(7) . . ?
O1 Cu1 N4 96.46(6) . 2_655 ?
O2 Cu1 N4 91.11(6) . 2_655 ?
N3 Cu1 N4 97.66(6) . 2_655 ?
N7 Cu1 N4 92.06(6) . 2_655 ?
C3 N1 C2 115.68(19) . . ?
C6 N2 N3 108.12(15) . . ?
C7 N3 N2 120.53(15) . . ?
C7 N3 Cu1 124.51(13) . . ?
N2 N3 Cu1 114.87(11) . . ?
C9 N4 C10 116.60(18) . . ?
C9 N4 Cu1 118.94(13) . 2_645 ?
C10 N4 Cu1 124.46(13) . 2_645 ?
C15 N5 C14 116.0(2) . . ?
C18 N6 N7 108.45(15) . . ?
C19 N7 N6 120.45(16) . . ?
C19 N7 Cu1 124.72(14) . . ?
N6 N7 Cu1 114.25(12) . . ?
C22 N8 C21 116.0(2) . . ?
C6 O1 Cu1 110.53(12) . . ?
C18 O2 Cu1 109.89(12) . . ?
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 C2 1.382(3) . ?
C1 C5 1.388(3) . ?
C2 N1 1.332(3) . ?
C3 N1 1.328(3) . ?
C3 C4 1.381(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.494(3) . ?
C6 O1 1.281(2) . ?
C6 N2 1.324(2) . ?
C7 N3 1.282(2) . ?
C7 C8 1.458(2) . ?
C8 C9 1.393(3) . ?
C8 C12 1.401(3) . ?
C9 N4 1.337(2) . ?
C10 N4 1.343(3) . ?
C10 C11 1.376(3) . ?
C11 C12 1.380(3) . ?
C13 C14 1.377(3) . ?
C13 C17 1.389(3) . ?
C14 N5 1.331(3) . ?
C15 N5 1.328(3) . ?
C15 C16 1.382(3) . ?
C16 C17 1.389(3) . ?
C17 C18 1.486(3) . ?
C18 O2 1.281(2) . ?
C18 N6 1.324(2) . ?
C19 N7 1.285(2) . ?
C19 C20 1.456(3) . ?
C20 C21 1.384(3) . ?
C20 C24 1.392(3) . ?
C21 N8 1.330(3) . ?
C22 N8 1.319(3) . ?
C22 C23 1.372(3) . ?
C23 C24 1.382(3) . ?
Cu1 O1 1.9459(13) . ?
Cu1 O2 1.9520(13) . ?
Cu1 N3 1.9536(15) . ?
Cu1 N7 1.9628(16) . ?
Cu1 N4 2.3411(16) 2_655 ?
N2 N3 1.395(2) . ?
N4 Cu1 2.3411(16) 2_645 ?
N6 N7 1.389(2) . ?
