#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:56:56 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179605 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/69/4506945.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_4506945
loop_
_publ_author_name
'Liu, Juan'
'Tan, Yan-Xi'
'Zhang, Jian'
_publ_section_title
;
 Redox Reaction Induced Structural Transformation among Three Copper
 Coordination Polymers
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5164
_journal_paper_doi               10.1021/cg301120b
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C43 H41 Cu3 N8 O10'
_chemical_formula_weight         1020.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2091(7)
_cell_length_b                   22.7532(16)
_cell_length_c                   23.0902(12)
_cell_measurement_reflns_used    1442
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0415
_cell_measurement_theta_min      2.3811
_cell_volume                     4838.2(6)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega 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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9761
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2087
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1481P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2755
_reflns_number_gt                2266
_reflns_number_total             4348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301120b_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4506945
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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 0.38884(11) 0.03282(5) 0.53264(4) 0.0658(5) Uani 1 1 d .
Cu2 Cu 0.26482(18) 0.2500 0.52734(5) 0.0623(5) Uani 1 2 d S
O1 O 0.3482(15) 0.2500 0.6991(3) 0.127(4) Uani 1 2 d S
O2 O 0.3832(11) 0.2500 0.6038(3) 0.082(3) Uani 1 2 d S
O3 O 0.0842(11) 0.2500 0.4738(3) 0.086(3) Uani 1 2 d S
O4 O -0.1568(15) 0.2500 0.4760(5) 0.155(6) Uani 1 2 d S
O5 O 0.4626(7) 0.0972(3) 0.4627(2) 0.0750(18) Uani 1 1 d .
O6 O 0.3073(7) 0.1513(2) 0.5119(2) 0.0660(16) Uani 1 1 d .
O7 O 0.332(2) 0.1288(11) 0.1639(11) 0.55(2) Uiso 1 1 d D
N1 N 0.1075(15) 0.2500 0.5833(4) 0.072(3) Uani 1 2 d S
N2 N 0.4172(10) 0.2500 0.4672(3) 0.050(2) Uani 1 2 d S
N3 N 0.4913(7) 0.0518(3) 0.6027(2) 0.0546(17) Uani 1 1 d .
N4 N 0.2599(6) 0.0057(3) 0.9878(2) 0.0529(17) Uani 1 1 d .
N5 N 0.5555(17) 0.1445(6) 0.1801(6) 0.195(6) Uiso 1 1 d D
C1 C 0.1394(19) 0.2500 0.6402(6) 0.076(4) Uani 1 2 d S
C2 C 0.024(2) 0.2500 0.6812(6) 0.093(5) Uani 1 2 d S
H2A H 0.0419 0.2500 0.7209 0.112 Uiso 1 2 calc SR
C3 C -0.112(2) 0.2500 0.6597(7) 0.111(6) Uani 1 2 d S
H3A H -0.1887 0.2500 0.6860 0.133 Uiso 1 2 calc SR
C4 C -0.145(2) 0.2500 0.6040(7) 0.101(5) Uani 1 2 d S
H4A H -0.2411 0.2500 0.5914 0.121 Uiso 1 2 calc SR
C5 C -0.027(2) 0.2500 0.5641(7) 0.091(4) Uani 1 2 d S
C6 C 0.294(2) 0.2500 0.6495(5) 0.084(5) Uani 1 2 d S
C7 C -0.042(2) 0.2500 0.4997(6) 0.094(5) Uani 1 2 d S
C8 C 0.4640(8) 0.1978(3) 0.4460(3) 0.0517(19) Uani 1 1 d .
C9 C 0.5577(10) 0.1961(4) 0.4012(4) 0.075(3) Uani 1 1 d .
H9A H 0.5904 0.1606 0.3861 0.090 Uiso 1 1 calc R
C10 C 0.6039(15) 0.2500 0.3781(6) 0.101(5) Uani 1 2 d S
H10A H 0.6671 0.2500 0.3467 0.122 Uiso 1 2 calc SR
C11 C 0.4055(10) 0.1442(3) 0.4766(4) 0.056(2) Uani 1 1 d .
C12 C 0.5506(10) 0.0101(4) 0.6356(3) 0.066(2) Uani 1 1 d .
H12A H 0.5509 -0.0284 0.6222 0.079 Uiso 1 1 calc R
C13 C 0.6118(9) 0.0222(4) 0.6889(3) 0.063(2) Uani 1 1 d .
H13A H 0.6523 -0.0084 0.7102 0.075 Uiso 1 1 calc R
C14 C 0.6143(8) 0.0766(4) 0.7108(3) 0.0497(19) Uani 1 1 d .
C15 C 0.5572(8) 0.1198(4) 0.6759(3) 0.059(2) Uani 1 1 d .
H15A H 0.5596 0.1587 0.6882 0.070 Uiso 1 1 calc R
C16 C 0.4965(8) 0.1061(4) 0.6232(3) 0.057(2) Uani 1 1 d .
H16A H 0.4574 0.1364 0.6009 0.068 Uiso 1 1 calc R
C17 C 0.6638(9) 0.0887(4) 0.7713(3) 0.066(2) Uani 1 1 d .
H17A H 0.6896 0.1298 0.7750 0.079 Uiso 1 1 calc R
H17B H 0.7494 0.0654 0.7797 0.079 Uiso 1 1 calc R
C18 C 0.5441(9) 0.0737(4) 0.8142(3) 0.063(2) Uani 1 1 d .
H18A H 0.4615 0.0991 0.8068 0.076 Uiso 1 1 calc R
H18B H 0.5131 0.0335 0.8075 0.076 Uiso 1 1 calc R
C19 C 0.5870(9) 0.0799(5) 0.8768(3) 0.070(3) Uani 1 1 d .
H19A H 0.6015 0.1212 0.8857 0.085 Uiso 1 1 calc R
H19B H 0.6781 0.0596 0.8833 0.085 Uiso 1 1 calc R
C20 C 0.2783(9) 0.0630(4) 0.9835(3) 0.065(2) Uani 1 1 d .
H20A H 0.2179 0.0873 1.0051 0.078 Uiso 1 1 calc R
C21 C 0.3808(9) 0.0886(4) 0.9491(3) 0.064(2) Uani 1 1 d .
H21A H 0.3887 0.1293 0.9479 0.077 Uiso 1 1 calc R
C22 C 0.4717(9) 0.0548(4) 0.9165(3) 0.061(2) Uani 1 1 d .
C23 C 0.4527(9) -0.0057(4) 0.9208(3) 0.061(2) Uani 1 1 d .
H23A H 0.5116 -0.0308 0.8994 0.074 Uiso 1 1 calc R
C24 C 0.3493(9) -0.0282(4) 0.9559(3) 0.058(2) Uani 1 1 d .
H24A H 0.3395 -0.0689 0.9582 0.070 Uiso 1 1 calc R
C25 C 0.438(2) 0.1541(10) 0.1383(9) 0.138(9) Uiso 0.50 1 d PD
H25A H 0.4396 0.1733 0.1028 0.166 Uiso 0.50 1 calc PR
C26 C 0.581(2) 0.1113(9) 0.2337(8) 0.118(8) Uiso 0.50 1 d PD
H26A H 0.6778 0.1190 0.2475 0.177 Uiso 0.50 1 calc PR
H26B H 0.5708 0.0700 0.2261 0.177 Uiso 0.50 1 calc PR
H26C H 0.5121 0.1231 0.2626 0.177 Uiso 0.50 1 calc PR
C27 C 0.688(2) 0.1660(10) 0.1531(9) 0.123(8) Uiso 0.50 1 d PD
H27A H 0.7684 0.1604 0.1791 0.185 Uiso 0.50 1 calc PR
H27B H 0.6781 0.2071 0.1445 0.185 Uiso 0.50 1 calc PR
H27C H 0.7057 0.1447 0.1179 0.185 Uiso 0.50 1 calc PR
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'
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'
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_1
_geom_angle_site_symmetry_3
N3 Cu1 N4 154.6(3) . 2_554
N3 Cu1 O5 107.7(3) . .
N4 Cu1 O5 97.1(2) 2_554 .
N3 Cu1 Cu1 101.7(2) . 5_656
N4 Cu1 Cu1 89.36(19) 2_554 5_656
O5 Cu1 Cu1 75.94(16) . 5_656
N1 Cu2 N2 177.1(4) . .
N1 Cu2 O3 78.4(4) . .
N2 Cu2 O3 98.7(3) . .
N1 Cu2 O2 80.0(5) . .
N2 Cu2 O2 103.0(4) . .
O3 Cu2 O2 158.3(4) . .
N1 Cu2 O6 103.26(16) . 8_565
N2 Cu2 O6 76.75(16) . 8_565
O3 Cu2 O6 92.52(16) . 8_565
O2 Cu2 O6 92.42(15) . 8_565
N1 Cu2 O6 103.26(17) . .
N2 Cu2 O6 76.75(16) . .
O3 Cu2 O6 92.52(16) . .
O2 Cu2 O6 92.42(15) . .
O6 Cu2 O6 153.5(3) 8_565 .
C6 O2 Cu2 110.5(9) . .
C7 O3 Cu2 116.1(9) . .
C11 O5 Cu1 104.1(6) . .
C11 O6 Cu2 110.9(5) . .
C5 N1 C1 122.4(13) . .
C5 N1 Cu2 118.5(9) . .
C1 N1 Cu2 119.1(11) . .
C8 N2 C8 122.5(10) . 8_565
C8 N2 Cu2 118.7(5) . .
C8 N2 Cu2 118.7(5) 8_565 .
C16 N3 C12 116.5(7) . .
C16 N3 Cu1 121.8(6) . .
C12 N3 Cu1 121.4(6) . .
C20 N4 C24 116.5(7) . .
C20 N4 Cu1 125.5(6) . 2
C24 N4 Cu1 117.9(6) . 2
C27 N5 C25 106.9(19) . .
C27 N5 C26 113.4(17) . .
C25 N5 C26 138.5(19) . .
N1 C1 C2 119.1(16) . .
N1 C1 C6 111.2(13) . .
C2 C1 C6 129.7(14) . .
C3 C2 C1 116.7(14) . .
C3 C2 H2A 121.7 . .
C1 C2 H2A 121.7 . .
C4 C3 C2 124.8(18) . .
C4 C3 H3A 117.6 . .
C2 C3 H3A 117.6 . .
C3 C4 C5 117.0(18) . .
C3 C4 H4A 121.5 . .
C5 C4 H4A 121.5 . .
N1 C5 C4 119.9(16) . .
N1 C5 C7 115.1(15) . .
C4 C5 C7 125.0(18) . .
O1 C6 O2 118.8(17) . .
O1 C6 C1 121.9(15) . .
O2 C6 C1 119.2(11) . .
O4 C7 O3 125.3(14) . .
O4 C7 C5 122.8(18) . .
O3 C7 C5 111.9(16) . .
C9 C8 N2 120.3(8) . .
C9 C8 C11 124.5(8) . .
N2 C8 C11 115.2(7) . .
C8 C9 C10 117.5(9) . .
C8 C9 H9A 121.2 . .
C10 C9 H9A 121.2 . .
C9 C10 C9 121.9(12) 8_565 .
C9 C10 H10A 119.1 8_565 .
C9 C10 H10A 119.1 . .
O6 C11 O5 127.0(8) . .
O6 C11 C8 117.8(7) . .
O5 C11 C8 115.2(8) . .
N3 C12 C13 122.3(8) . .
N3 C12 H12A 118.9 . .
C13 C12 H12A 118.9 . .
C14 C13 C12 121.9(8) . .
C14 C13 H13A 119.1 . .
C12 C13 H13A 119.1 . .
C13 C14 C15 115.6(7) . .
C13 C14 C17 121.9(8) . .
C15 C14 C17 122.2(8) . .
C14 C15 C16 120.9(8) . .
C14 C15 H15A 119.5 . .
C16 C15 H15A 119.5 . .
N3 C16 C15 122.7(8) . .
N3 C16 H16A 118.6 . .
C15 C16 H16A 118.6 . .
C14 C17 C18 110.3(6) . .
C14 C17 H17A 109.6 . .
C18 C17 H17A 109.6 . .
C14 C17 H17B 109.6 . .
C18 C17 H17B 109.6 . .
H17A C17 H17B 108.1 . .
C19 C18 C17 114.5(7) . .
C19 C18 H18A 108.6 . .
C17 C18 H18A 108.6 . .
C19 C18 H18B 108.6 . .
C17 C18 H18B 108.6 . .
H18A C18 H18B 107.6 . .
C18 C19 C22 111.2(7) . .
C18 C19 H19A 109.4 . .
C22 C19 H19A 109.4 . .
C18 C19 H19B 109.4 . .
C22 C19 H19B 109.4 . .
H19A C19 H19B 108.0 . .
N4 C20 C21 123.7(8) . .
N4 C20 H20A 118.2 . .
C21 C20 H20A 118.2 . .
C22 C21 C20 120.4(8) . .
C22 C21 H21A 119.8 . .
C20 C21 H21A 119.8 . .
C21 C22 C23 116.1(7) . .
C21 C22 C19 123.5(8) . .
C23 C22 C19 120.4(8) . .
C24 C23 C22 120.5(8) . .
C24 C23 H23A 119.7 . .
C22 C23 H23A 119.7 . .
N4 C24 C23 122.7(8) . .
N4 C24 H24A 118.6 . .
C23 C24 H24A 118.6 . .
O7 C25 N5 101.1(18) . .
O7 C25 H25A 129.4 . .
N5 C25 H25A 129.4 . .
N5 C26 H26A 109.5 . .
N5 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
N5 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
N5 C27 H27A 109.5 . .
N5 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
N5 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N3 1.923(6) .
Cu1 N4 1.928(6) 2_554
Cu1 O5 2.285(6) .
Cu1 Cu1 2.949(2) 5_656
Cu2 N1 1.942(11) .
Cu2 N2 1.973(9) .
Cu2 O3 2.072(9) .
Cu2 O2 2.074(8) .
Cu2 O6 2.308(5) 8_565
Cu2 O6 2.308(5) .
O1 C6 1.250(14) .
O2 C6 1.336(16) .
O3 C7 1.308(19) .
O4 C7 1.19(2) .
O5 C11 1.233(9) .
O6 C11 1.228(9) .
O7 C25 1.273(10) .
N1 C5 1.316(18) .
N1 C1 1.345(15) .
N2 C8 1.356(8) .
N2 C8 1.356(8) 8_565
N3 C16 1.324(10) .
N3 C12 1.332(10) .
N4 C20 1.319(11) .
N4 C24 1.347(10) .
N4 Cu1 1.928(6) 2
N5 C27 1.456(10) .
N5 C25 1.467(10) .
N5 C26 1.471(9) .
C1 C2 1.42(2) .
C1 C6 1.44(2) .
C2 C3 1.35(2) .
C2 H2A 0.9300 .
C3 C4 1.32(2) .
C3 H3A 0.9300 .
C4 C5 1.43(2) .
C4 H4A 0.9300 .
C5 C7 1.49(2) .
C8 C9 1.349(11) .
C8 C11 1.509(11) .
C9 C10 1.402(10) .
C9 H9A 0.9300 .
C10 C9 1.402(10) 8_565
C10 H10A 0.9300 .
C12 C13 1.381(10) .
C12 H12A 0.9300 .
C13 C14 1.338(11) .
C13 H13A 0.9300 .
C14 C15 1.375(10) .
C14 C17 1.494(9) .
C15 C16 1.376(9) .
C15 H15A 0.9300 .
C16 H16A 0.9300 .
C17 C18 1.522(10) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 C19 1.504(9) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C22 1.515(10) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 C21 1.364(11) .
C20 H20A 0.9300 .
C21 C22 1.364(11) .
C21 H21A 0.9300 .
C22 C23 1.391(12) .
C23 C24 1.351(11) .
C23 H23A 0.9300 .
C24 H24A 0.9300 .
C25 H25A 0.9300 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
