#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/03/2200354.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2200354
loop_
_publ_author_name
'Chuanpeng Cui'
'Jingcao Dai'
'Limin Wu'
'Wenxin Du'
'Xintao Wu'
_publ_section_title
;
 A tetranuclear copper complex,
 [Cu₄(μ₃-OH)₂(μ₂-OH)₂(phen)₄(H₂O)₂](NO₃)₄·2H₂O
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m198
_journal_page_last               m200
_journal_paper_doi               10.1107/S1600536801006018
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac
'[Cu4 (O H)4 (C10 H8 N2)4 (H2 O)2] (N O3)4, 2H2 O'
_chemical_formula_moiety         'C48 H32 Cu4 N8 O6 4+, 4N1 O3 1-, 2H2 O1'
_chemical_formula_sum            'C48 H36 Cu4 N12 O20'
_chemical_formula_weight         1355.04
_chemical_name_common
'[Cu(OH)~4~(C~12~H~8~N~2)~4~(H~2~O)~4~(NO~3~)~4~]'
_chemical_name_systematic
;
Diaquadi-μ₃-hydroxo-di-μ₂-hydroxo-tetraphenanthrolinetetracopper(II)
tetranitrate dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                111.0730(10)
_cell_angle_beta                 90.906(2)
_cell_angle_gamma                111.218(2)
_cell_formula_units_Z            1
_cell_length_a                   10.15040(10)
_cell_length_b                   11.9299(3)
_cell_length_c                   12.63370(10)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.75
_cell_volume                     1311.91(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1998)'
_computing_data_reduction        'SAINT (Siemens, 1998)'
_computing_molecular_graphics    'please provide'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .982
_diffrn_measured_fraction_theta_max .982
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0395
_diffrn_reflns_av_sigmaI/netI    .0986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6772
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  .816
_exptl_absorpt_correction_T_min  .597
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             684
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .12
_refine_diff_density_max         .764
_refine_diff_density_min         -.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.392
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.392
_refine_ls_R_factor_all          .1261
_refine_ls_R_factor_gt           .0688
_refine_ls_shift/su_max          .008
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1296
_reflns_number_gt                2762
_reflns_number_total             4544
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wn6011.cif
_cod_data_source_block           I
_cod_database_code               2200354
_cod_database_fobs_code          2200354
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 -.07137(8) -.20032(7) -.22381(7) .0364(3) Uani d . 1 . . Cu
Cu2 -.14418(8) -.00019(7) -.05315(7) .0344(3) Uani d . 1 . . Cu
N1 -.2437(5) .0087(5) .0859(4) .0319(13) Uani d . 1 . . N
N4 .0184(6) -.2146(5) -.3673(5) .0385(14) Uani d . 1 . . N
N2 -.2270(5) .1286(5) -.0570(5) .0345(14) Uani d . 1 . . N
N3 -.0024(5) -.3416(5) -.2306(5) .0317(13) Uani d . 1 . . N
N5 -.3649(8) -.1851(10) -.4818(7) .075(2) Uani d . 1 . . N
N6 -.2649(9) -.3516(6) .0738(7) .0555(18) Uani d . 1 . . N
O1 -.2986(5) -.3374(4) -.3010(4) .0545(15) Uani d . 1 . . O
O2 -.1000(4) -.0444(4) -.2066(3) .0375(12) Uani d . 1 . . O
H2A -.0943 -.0029 -.2572 .045 Uiso calc R 1 . . H
O3 -.0799(7) -.1384(6) -.0574(5) .0357(15) Uani d . 1 . . O
O4 -.3005(7) -.0855(6) -.3920(6) .0792(19) Uani d . 1 . . O
O5 -.3808(9) -.2949(8) -.4920(6) .122(3) Uani d . 1 . . O
O6 -.4296(9) -.1768(8) -.5602(7) .151(4) Uani d . 1 . . O
O7 -.3077(7) -.3558(6) -.0207(6) .095(2) Uani d . 1 . . O
O8 -.3485(7) -.3906(7) .1331(7) .109(3) Uani d . 1 . . O
O9 -.1363(7) -.3044(6) .1056(6) .095(2) Uani d . 1 . . O
O10 -.4166(6) -.5632(5) -.2601(5) .0904(19) Uani d . 1 . . O
C15 .1308(9) -.5131(8) -.2544(8) .057(3) Uani d . 1 . . C
C7 -.3895(7) .2288(6) .0337(6) .0382(18) Uani d . 1 . . C
C2 -.3346(8) -.0450(7) .2428(7) .045(2) Uani d . 1 . . C
C9 -.2824(8) .2743(7) -.1227(8) .046(2) Uani d . 1 . . C
C1 -.2501(7) -.0531(7) .1566(6) .0387(18) Uani d . 1 . . C
C22 .0276(9) -.1505(8) -.4352(7) .057(2) Uani d . 1 . . C
C20 .1858(9) -.2381(9) -.5420(8) .065(3) Uani d . 1 . . C
C8 -.3689(8) .2925(7) -.0442(7) .046(2) Uani d . 1 . . C
C14 .0467(8) -.4945(7) -.1714(8) .051(2) Uani d . 1 . . C
C18 .2473(9) -.3962(8) -.4876(7) .063(3) Uani d . 1 . . C
H10A .3038 -.4072 -.5446 .076 Uiso calc R 1 . . H
C19 .1765(7) -.3100(7) -.4740(7) .047(2) Uani d . 1 . . C
C16 .1477(7) -.4499(7) -.3311(7) .0429(19) Uani d . 1 . . C
C17 .2339(10) -.4609(10) -.4204(9) .066(3) Uani d . 1 . . C
C21 .1112(9) -.1581(8) -.5222(7) .070(3) Uani d . 1 . . C
H14A .1166 -.1095 -.5665 .084 Uiso calc R 1 . . H
C13 -.0180(8) -.4048(7) -.1621(7) .043(2) Uani d . 1 . . C
C6 -.4797(7) .2402(7) .1211(7) .043(2) Uani d . 1 . . C
C3 -.4167(8) .0293(7) .2580(7) .048(2) Uani d . 1 . . C
C10 -.2136(8) .1898(7) -.1279(7) .0428(19) Uani d . 1 . . C
C4 -.4121(6) .0963(6) .1830(6) .0357(17) Uani d . 1 . . C
C5 -.4882(8) .1784(7) .1930(7) .042(2) Uani d . 1 . . C
C24 .0779(7) -.3640(6) -.3145(6) .0346(17) Uani d . 1 . . C
C23 .0900(7) -.2957(6) -.3879(6) .0369(18) Uani d . 1 . . C
C12 -.3248(6) .0821(6) .0997(6) .0333(17) Uani d . 1 . . C
C11 -.3131(7) .1469(6) .0234(6) .0328(17) Uani d . 1 . . C
H13 -.342(6) -.091(6) .286(5) .04(2) Uiso d . 1 . . H
H12 -.143(6) .185(5) -.171(5) .023(17) Uiso d . 1 . . H
H11 -.482(7) .027(7) .317(6) .07(2) Uiso d . 1 . . H
H10 -.416(6) .340(6) -.041(5) .04(2) Uiso d . 1 . . H
H9 -.540(6) .189(6) .247(6) .04(2) Uiso d . 1 . . H
H8 .262(8) -.244(7) -.594(7) .10(3) Uiso d . 1 . . H
H6 -.072(6) -.393(6) -.100(5) .05(2) Uiso d . 1 . . H
H5 .033(6) -.531(6) -.115(5) .04(2) Uiso d . 1 . . H
H4 -.269(6) .312(5) -.170(5) .018(17) Uiso d . 1 . . H
H3 -.023(6) -.097(5) -.422(5) .034(19) Uiso d . 1 . . H
H2 -.527(7) .306(7) .128(6) .08(3) Uiso d . 1 . . H
H1 .169(10) -.570(9) -.263(8) .12(4) Uiso d . 1 . . H
H17 -.127(8) -.180(7) -.051(8) .05(3) Uiso d . 1 . . H
H16 -.194(8) -.118(7) .151(6) .09(3) Uiso d . 1 . . H
H15 .262(7) -.502(6) -.414(6) .03(2) Uiso d . 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Cu1 O3 . . 81.9(2) yes
O2 Cu1 N4 . . 95.8(2) yes
O3 Cu1 N4 . . 157.3(2) yes
O2 Cu1 N3 . . 169.30(19) yes
O3 Cu1 N3 . . 96.5(2) yes
N4 Cu1 N3 . . 81.6(2) yes
O2 Cu1 O1 . . 95.62(17) yes
O3 Cu1 O1 . . 102.1(2) yes
N4 Cu1 O1 . . 100.7(2) yes
N3 Cu1 O1 . . 95.06(18) yes
O2 Cu1 Cu2 . . 40.65(13) yes
O3 Cu1 Cu2 . . 42.09(17) yes
N4 Cu1 Cu2 . . 135.16(16) yes
N3 Cu1 Cu2 . . 138.57(17) yes
O1 Cu1 Cu2 . . 95.07(12) yes
O2 Cu2 O3 . . 82.1(2) yes
O2 Cu2 N2 . . 96.9(2) yes
O3 Cu2 N2 . . 174.9(2) yes
O2 Cu2 N1 . . 164.44(19) yes
O3 Cu2 N1 . . 97.7(2) yes
N2 Cu2 N1 . . 81.9(2) yes
O2 Cu2 O3 . 2 101.9(2) yes
O3 Cu2 O3 . 2 83.7(3) yes
N2 Cu2 O3 . 2 101.4(2) yes
N1 Cu2 O3 . 2 93.6(2) yes
O2 Cu2 Cu1 . . 40.60(11) yes
O3 Cu2 Cu1 . . 42.39(18) yes
N2 Cu2 Cu1 . . 135.62(17) yes
N1 Cu2 Cu1 . . 134.52(15) yes
O3 Cu2 Cu1 2 . 100.32(13) yes
C1 N1 C12 . . 117.8(6) yes
C1 N1 Cu2 . . 129.8(4) yes
C12 N1 Cu2 . . 112.1(4) yes
C22 N4 C23 . . 117.5(7) ?
C22 N4 Cu1 . . 130.2(5) ?
C23 N4 Cu1 . . 112.1(5) ?
C10 N2 C11 . . 118.4(6) ?
C10 N2 Cu2 . . 129.4(5) ?
C11 N2 Cu2 . . 112.1(5) ?
C13 N3 C24 . . 118.6(6) ?
C13 N3 Cu1 . . 129.0(5) ?
C24 N3 Cu1 . . 112.3(5) ?
O5 N5 O6 . . 116.4(10) ?
O5 N5 O4 . . 123.2(8) ?
O6 N5 O4 . . 120.0(10) ?
O9 N6 O8 . . 121.4(8) ?
O9 N6 O7 . . 117.1(8) ?
O8 N6 O7 . . 121.4(9) ?
Cu1 O2 Cu2 . . 98.75(19) yes
Cu1 O2 H2A . . 130.6 ?
Cu2 O2 H2A . . 130.6 ?
Cu2 O3 Cu1 . . 95.5(3) yes
Cu2 O3 Cu2 . 2 96.3(3) yes
Cu1 O3 Cu2 . 2 111.9(3) yes
Cu2 O3 H17 . . 109(9) ?
Cu1 O3 H17 . . 107(9) ?
Cu2 O3 H17 2 . 131(9) ?
C14 C15 C16 . . 121.4(8) ?
C14 C15 H1 . . 119(7) ?
C16 C15 H1 . . 120(7) ?
C8 C7 C11 . . 116.0(7) ?
C8 C7 C6 . . 125.9(7) ?
C11 C7 C6 . . 118.1(7) ?
C3 C2 C1 . . 120.2(8) ?
C3 C2 H13 . . 118(4) ?
C1 C2 H13 . . 122(4) ?
C8 C9 C10 . . 119.2(8) ?
C8 C9 H4 . . 122(4) ?
C10 C9 H4 . . 119(4) ?
N1 C1 C2 . . 122.5(7) ?
N1 C1 H16 . . 124(4) ?
C2 C1 H16 . . 114(4) ?
N4 C22 C21 . . 123.1(8) ?
N4 C22 H3 . . 117(4) ?
C21 C22 H3 . . 120(4) ?
C21 C20 C19 . . 119.2(8) ?
C21 C20 H8 . . 128(5) ?
C19 C20 H8 . . 112(4) ?
C9 C8 C7 . . 120.8(7) ?
C9 C8 H10 . . 122(5) ?
C7 C8 H10 . . 117(5) ?
C15 C14 C13 . . 117.7(9) ?
C15 C14 H5 . . 126(4) ?
C13 C14 H5 . . 116(4) ?
C17 C18 C19 . . 120.7(8) ?
C17 C18 H10A . . 119.6 ?
C19 C18 H10A . . 119.6 ?
C20 C19 C23 . . 117.2(7) ?
C20 C19 C18 . . 123.9(8) ?
C23 C19 C18 . . 118.9(8) ?
C24 C16 C15 . . 116.0(8) ?
C24 C16 C17 . . 117.8(8) ?
C15 C16 C17 . . 126.2(8) ?
C18 C17 C16 . . 122.9(9) ?
C18 C17 H15 . . 135(7) ?
C16 C17 H15 . . 102(7) ?
C20 C21 C22 . . 119.7(9) ?
C20 C21 H14A . . 120.2 ?
C22 C21 H14A . . 120.2 ?
N3 C13 C14 . . 122.8(8) ?
N3 C13 H6 . . 123(4) ?
C14 C13 H6 . . 114(4) ?
C5 C6 C7 . . 121.1(7) ?
C5 C6 H2 . . 124(4) ?
C7 C6 H2 . . 114(4) ?
C2 C3 C4 . . 118.3(7) ?
C2 C3 H11 . . 117(4) ?
C4 C3 H11 . . 124(4) ?
N2 C10 C9 . . 123.0(8) ?
N2 C10 H12 . . 114(4) ?
C9 C10 H12 . . 122(4) ?
C12 C4 C5 . . 119.7(7) ?
C12 C4 C3 . . 117.1(7) ?
C5 C4 C3 . . 123.1(7) ?
C6 C5 C4 . . 121.1(7) ?
C6 C5 H9 . . 120(4) ?
C4 C5 H9 . . 119(4) ?
N3 C24 C16 . . 123.4(7) ?
N3 C24 C23 . . 116.9(6) ?
C16 C24 C23 . . 119.7(7) ?
N4 C23 C19 . . 123.4(7) ?
N4 C23 C24 . . 116.5(6) ?
C19 C23 C24 . . 120.1(7) ?
N1 C12 C4 . . 123.9(7) ?
N1 C12 C11 . . 115.7(6) ?
C4 C12 C11 . . 120.4(6) ?
N2 C11 C12 . . 117.8(6) ?
N2 C11 C7 . . 122.5(7) ?
C12 C11 C7 . . 119.7(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O2 . 1.922(4) yes
Cu1 O3 . 1.977(6) yes
Cu1 N4 . 2.022(6) yes
Cu1 N3 . 2.022(5) yes
Cu1 O1 . 2.235(4) yes
Cu1 Cu2 . 2.9191(10) yes
Cu2 O2 . 1.924(4) yes
Cu2 O3 . 1.966(6) yes
Cu2 N2 . 2.013(5) yes
Cu2 N1 . 2.029(5) yes
Cu2 O3 2 2.318(6) yes
N1 C1 . 1.337(8) ?
N1 C12 . 1.375(7) ?
N4 C22 . 1.323(9) ?
N4 C23 . 1.366(8) ?
N2 C10 . 1.326(9) ?
N2 C11 . 1.360(8) ?
N3 C13 . 1.316(9) ?
N3 C24 . 1.357(8) ?
N5 O5 . 1.218(9) ?
N5 O6 . 1.233(8) ?
N5 O4 . 1.253(9) ?
N6 O9 . 1.213(7) ?
N6 O8 . 1.217(9) ?
N6 O7 . 1.241(8) ?
O2 H2A . .9300 ?
O3 Cu2 2 2.318(6) yes
O3 H17 . .58(7) ?
C15 C14 . 1.369(11) ?
C15 C16 . 1.405(11) ?
C15 H1 . .87(8) ?
C7 C8 . 1.421(10) ?
C7 C11 . 1.425(8) ?
C7 C6 . 1.446(10) ?
C2 C3 . 1.392(10) ?
C2 C1 . 1.394(10) ?
C2 H13 . .89(6) ?
C9 C8 . 1.345(11) ?
C9 C10 . 1.404(9) ?
C9 H4 . .85(5) ?
C1 H16 . 1.10(7) ?
C22 C21 . 1.396(11) ?
C22 H3 . .93(5) ?
C20 C21 . 1.379(11) ?
C20 C19 . 1.399(11) ?
C20 H8 . 1.02(8) ?
C8 H10 . .85(5) ?
C14 C13 . 1.418(9) ?
C14 H5 . .96(6) ?
C18 C17 . 1.317(13) ?
C18 C19 . 1.420(10) ?
C18 H10A . .9300 ?
C19 C23 . 1.411(9) ?
C16 C24 . 1.404(8) ?
C16 C17 . 1.435(13) ?
C17 H15 . .68(5) ?
C21 H14A . .9300 ?
C13 H6 . .97(6) ?
C6 C5 . 1.347(10) ?
C6 H2 . 1.04(7) ?
C3 C4 . 1.435(10) ?
C3 H11 . 1.01(7) ?
C10 H12 . .91(5) ?
C4 C12 . 1.389(9) ?
C4 C5 . 1.426(9) ?
C5 H9 . .87(6) ?
C24 C23 . 1.419(9) ?
C12 C11 . 1.420(9) ?
