#------------------------------------------------------------------------------
#$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $
#$Revision: 19 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1100140.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_1100140
loop_
_publ_author_name
       'Jorge A. R. Navarro'
       'Elisa Barea'
       'Miguel Quiros'
       'Juan M. Salas'
_journal_name_full 'Journal of the Chemical Society. Dalton Transactions'
_journal_volume         ?
_journal_page_first     1743
_journal_page_last      1746
_journal_year           2005
_publ_section_title
;
Heteroleptic Pyrimidine-2-olate and 4,4'-bipyridine
Copper(II) Layered Metal-organic Frameworks with Swelling Properties
;
_chemical_name_systematic
;
?
;
_chemical_name_common
(Cu3Cl2(OH)3(2-pymo)(4,4'-bpy)1.5)n(NO3)n.6.25nH2O
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H41.50 Cl2 Cu3 N9 O12.25'
_chemical_formula_weight         1033.78
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n 2'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a                   17.076(3)
_cell_length_b                   19.341(3)
_cell_length_c                   13.481(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4452.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2098
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.7
_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2110
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6260
_exptl_absorpt_correction_T_max  0.9297
_exptl_absorpt_process_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27660
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_sigmaI/netI    0.1066
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         28.44
_reflns_number_total             8792
_reflns_number_gt                6423
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.38(3)
_refine_ls_number_reflns         8792
_refine_ls_number_parameters     532
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.2176
_refine_ls_wR_factor_gt          0.2010
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.001
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
Cu1 Cu 0.74340(8) 0.39747(6) 0.5000 0.0191(3) Uani 1 1 d . . .
Cu2 Cu 0.78112(7) 0.53035(6) 0.63488(15) 0.0193(3) Uani 1 1 d . . .
Cu3 Cu 0.70975(7) 0.26090(6) 0.36270(15) 0.0178(3) Uani 1 1 d . . .
Cl2 Cl 0.59672(18) 0.33689(14) 0.4426(2) 0.0335(7) Uani 1 1 d . . .
Cl3 Cl 0.88731(15) 0.44800(12) 0.5623(2) 0.0218(5) Uani 1 1 d . . .
O2 O 0.6993(4) 0.4752(4) 0.5766(6) 0.0242(17) Uani 1 1 d . . .
O3 O 0.7847(4) 0.3205(4) 0.4245(5) 0.0206(16) Uani 1 1 d . . .
N1P N 0.6363(5) 0.1969(4) 0.2968(6) 0.0200(19) Uani 1 1 d . . .
C2P C 0.6795(6) 0.1463(6) 0.2496(8) 0.021(2) Uani 1 1 d . . .
O2P O 0.7518(4) 0.1468(4) 0.2498(6) 0.0212(14) Uani 1 1 d . . .
N3P N 0.6392(5) 0.0939(4) 0.1974(7) 0.0214(19) Uani 1 1 d . . .
C4P C 0.5631(7) 0.0941(5) 0.1939(10) 0.031(3) Uani 1 1 d . . .
H4P H 0.5368 0.0591 0.1574 0.037 Uiso 1 1 d R . .
C5P C 0.5198(7) 0.1449(7) 0.2394(11) 0.038(3) Uani 1 1 d . . .
H5P H 0.4642 0.1450 0.2375 0.045 Uiso 1 1 d R . .
C6P C 0.5602(6) 0.1964(5) 0.2919(9) 0.026(2) Uani 1 1 d . . .
H6P H 0.5315 0.2319 0.3243 0.032 Uiso 1 1 d R . .
N11 N 0.7471(5) 0.4572(4) 0.3744(7) 0.0207(19) Uani 1 1 d . . .
C12 C 0.6874(6) 0.4976(5) 0.3478(8) 0.021(2) Uani 1 1 d . . .
H12 H 0.6409 0.4968 0.3865 0.025 Uiso 1 1 d R . .
C13 C 0.6906(6) 0.5401(5) 0.2672(8) 0.020(2) Uani 1 1 d . . .
H13 H 0.6471 0.5683 0.2504 0.024 Uiso 1 1 d R . .
C14 C 0.7563(7) 0.5422(5) 0.2103(8) 0.023(2) Uani 1 1 d . . .
C15 C 0.8195(6) 0.4990(5) 0.2360(8) 0.019(2) Uani 1 1 d . . .
H15 H 0.8656 0.4977 0.1966 0.023 Uiso 1 1 d R . .
C16 C 0.8120(6) 0.4577(5) 0.3201(8) 0.022(2) Uani 1 1 d . . .
H16 H 0.8547 0.4292 0.3392 0.026 Uiso 1 1 d R . .
N21 N 0.7385(5) 0.3365(4) 0.6230(7) 0.024(2) Uani 1 1 d . . .
C22 C 0.6760(7) 0.3323(5) 0.6818(8) 0.023(2) Uani 1 1 d . . .
H22 H 0.6324 0.3610 0.6670 0.027 Uiso 1 1 d R . .
C23 C 0.6703(7) 0.2885(5) 0.7618(8) 0.026(2) Uani 1 1 d . . .
H23 H 0.6227 0.2852 0.7979 0.032 Uiso 1 1 d R . .
C24 C 0.7351(7) 0.2494(5) 0.7895(8) 0.020(2) Uani 1 1 d . . .
C25 C 0.8011(7) 0.2537(5) 0.7295(10) 0.028(3) Uani 1 1 d . . .
H25 H 0.8456 0.2260 0.7440 0.033 Uiso 1 1 d R . .
C26 C 0.8027(7) 0.2973(5) 0.6480(9) 0.024(2) Uani 1 1 d . . .
H26 H 0.8488 0.3003 0.6088 0.029 Uiso 1 1 d R . .
N31 N 0.7741(5) 0.6000(4) 0.5212(6) 0.022(2) Uani 1 1 d . . .
C32 C 0.8356(7) 0.6145(5) 0.4675(9) 0.032(3) Uani 1 1 d . . .
H32 H 0.8832 0.5912 0.4819 0.038 Uiso 1 1 d R . .
C33 C 0.8357(7) 0.6626(6) 0.3919(8) 0.030(3) Uani 1 1 d . . .
H33 H 0.8812 0.6698 0.3527 0.037 Uiso 1 1 d R . .
C34 C 0.7690(7) 0.7000(5) 0.3729(9) 0.025(2) Uani 1 1 d . . .
C35 C 0.7032(7) 0.6840(5) 0.4311(8) 0.026(2) Uani 1 1 d . . .
H35 H 0.6546 0.7065 0.4194 0.031 Uiso 1 1 d R . .
C36 C 0.7090(6) 0.6359(5) 0.5044(9) 0.022(2) Uani 1 1 d . . .
H36 H 0.6647 0.6272 0.5452 0.027 Uiso 1 1 d R . .
N41 N 0.7659(5) 0.4832(4) 0.7689(7) 0.0213(19) Uani 1 1 d . . .
C42 C 0.6987(7) 0.4784(6) 0.8123(9) 0.033(3) Uani 1 1 d . . .
H42 H 0.6550 0.4985 0.7797 0.040 Uiso 1 1 d R . .
C43 C 0.6855(8) 0.4468(6) 0.9038(9) 0.037(3) Uani 1 1 d . . .
H43 H 0.6343 0.4446 0.9311 0.045 Uiso 1 1 d R . .
C44 C 0.7482(7) 0.4177(5) 0.9528(8) 0.022(2) Uani 1 1 d . . .
C45 C 0.8220(8) 0.4248(7) 0.9093(10) 0.040(3) Uani 1 1 d . . .
H45 H 0.8676 0.4090 0.9426 0.048 Uiso 1 1 d R . .
C46 C 0.8278(8) 0.4565(7) 0.8195(9) 0.039(3) Uani 1 1 d . . .
H46 H 0.8782 0.4593 0.7898 0.046 Uiso 1 1 d R . .
N51 N 0.7218(5) 0.1893(4) 0.4736(6) 0.0184(19) Uani 1 1 d . . .
C52 C 0.6616(7) 0.1740(5) 0.5324(8) 0.025(2) Uani 1 1 d . . .
H52 H 0.6138 0.1982 0.5227 0.030 Uiso 1 1 d R . .
C53 C 0.6646(6) 0.1256(5) 0.6076(8) 0.025(2) Uani 1 1 d . . .
H53 H 0.6197 0.1155 0.6467 0.030 Uiso 1 1 d R . .
C54 C 0.7361(6) 0.0916(5) 0.6246(8) 0.019(2) Uani 1 1 d . . .
C55 C 0.7971(6) 0.1053(5) 0.5625(9) 0.026(2) Uani 1 1 d . . .
H55 H 0.8449 0.0808 0.5701 0.032 Uiso 1 1 d R . .
C56 C 0.7898(6) 0.1547(5) 0.4869(8) 0.020(2) Uani 1 1 d . . .
H56 H 0.8334 0.1642 0.4453 0.024 Uiso 1 1 d R . .
N61 N 0.7206(5) 0.3130(4) 0.2303(7) 0.0197(18) Uani 1 1 d . . .
C62 C 0.7841(8) 0.3073(7) 0.1773(10) 0.040(3) Uani 1 1 d . . .
H62 H 0.8250 0.2790 0.2023 0.048 Uiso 1 1 d R . .
C63 C 0.7957(8) 0.3385(6) 0.0885(10) 0.040(3) Uani 1 1 d . . .
H63 H 0.8432 0.3313 0.0535 0.048 Uiso 1 1 d R . .
C64 C 0.7393(7) 0.3818(5) 0.0488(9) 0.024(2) Uani 1 1 d . . .
C65 C 0.6712(7) 0.3871(7) 0.1064(9) 0.037(3) Uani 1 1 d . . .
H65 H 0.6296 0.4159 0.0844 0.044 Uiso 1 1 d R . .
C66 C 0.6643(7) 0.3524(6) 0.1931(9) 0.037(3) Uani 1 1 d . . .
H66 H 0.6172 0.3566 0.2300 0.044 Uiso 1 1 d R . .
N1N N 0.996(2) 0.4504(9) 0.0161(15) 0.122(14) Uiso 0.50 1 d PD . .
O1N O 1.003(2) 0.4866(12) -0.0568(12) 0.071(7) Uiso 0.50 1 d PD . .
O2N O 0.988(3) 0.3879(9) 0.007(2) 0.175(18) Uiso 0.50 1 d PD . .
O3N O 0.9832(17) 0.4764(11) 0.0971(13) 0.099(9) Uiso 0.50 1 d PD . .
N2N N 0.493(2) 0.3580(14) 0.0239(19) 0.119(14) Uiso 0.50 1 d PD . .
O4N O 0.4780(16) 0.3393(12) 0.108(2) 0.089(8) Uiso 0.50 1 d PD . .
O5N O 0.487(3) 0.4194(17) 0.001(3) 0.179(17) Uiso 0.50 1 d PD . .
O6N O 0.498(7) 0.315(2) -0.042(3) 0.57(8) Uiso 0.50 1 d PD . .
O1W O 1.0000 0.5000 0.3946(10) 0.048(3) Uani 1 2 d S . .
O2W O 0.4637(7) 0.2677(6) 0.5684(11) 0.085(4) Uani 1 1 d . . .
O3W O 0.9099(7) 0.1581(10) 0.2336(10) 0.114(6) Uani 1 1 d . . .
O4W O 0.9986(8) 0.3807(9) 0.2488(14) 0.129(7) Uani 1 1 d . . .
O5W O 0.5000 0.5000 0.163(2) 0.089(8) Uiso 0.70 2 d SP . .
O6W O 0.9410(13) 0.2833(12) 0.3806(18) 0.117(8) Uiso 0.70 1 d P . .
O7W O 0.4887(15) 0.4352(13) 0.337(2) 0.138(9) Uiso 0.70 1 d P . .
O8W O 0.9713(14) 0.3666(12) 0.066(2) 0.071(6) Uiso 0.50 1 d P . .
O9W O 0.525(7) 0.512(6) 0.603(5) 0.36(5) Uiso 0.50 1 d P . .