#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:48:10 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178978 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/01/4120100.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_4120100
loop_
_publ_author_name
'Witold M. Bloch'
'Ravichandar Babarao'
'Matthew R. Hill'
'Christian J. Doonan'
'Christopher J. Sumby'
_publ_contact_author_address
;School of Chemistry & Physics
The University of Adelaide
Adelaide
SA 5005
Australia
;
_publ_contact_author_email       christopher.sumby@adelaide.edu.au
_publ_contact_author_fax         '+61 8 83134358'
_publ_contact_author_name        'Christopher Sumby'
_publ_contact_author_phone       '+61 8 83137406'
_publ_section_title
;
 Post-synthetic Structural Processing in a Metal-Organic Framework
 Material as a Mechanism for Exceptional CO2/N2 Selectivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10441
_journal_page_last               10448
_journal_paper_doi               10.1021/ja4032049
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C21 H16 Cu N4 O5'
_chemical_formula_weight         467.92
_chemical_name_common            '[Cu(bcppm)H2O]-pdes'
_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                   9.6611(4)
_cell_length_b                   20.3319(7)
_cell_length_c                   13.6276(5)
_cell_measurement_reflns_used    3838
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2595
_cell_measurement_theta_min      2.4944
_cell_volume                     2676.85(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'X-Seed (Barbour, 2003)'
_computing_publication_material  'CIFTAB (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
  1 omega   -6.00   56.00   1.0000   43.1400
omega____ theta____ kappa____ phi______ frames
    -       18.8463   37.0000  -90.0000 62

  2 omega   67.00   94.00   1.0000   43.1400
omega____ theta____ kappa____ phi______ frames
    -       18.8463 -159.0000  -56.0000 27

  3 omega  -82.00  -21.00   1.0000   43.1400
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -77.0000  150.0000 61

  4 omega  -98.00  -35.00   1.0000   43.1400
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  179.0000  -60.0000 63

  5 omega  -92.00    8.00   1.0000   43.1400
omega____ theta____ kappa____ phi______ frames
    -      -19.6276  -37.0000  -60.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15988
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       Block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0398
_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)+(0.0575P)²+0.4921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                2615
_reflns_number_total             3364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4032049_si_002_1.cif
_cod_data_source_block           '[Cu(bcppm)H2O]-pdes'
_cod_database_code               4120100
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.35201(4) 0.7500 0.23522(3) 0.01454(14) Uani 1 2 d S . .
O28 O 0.20265(17) 1.17890(7) -0.17624(12) 0.0202(4) Uani 1 1 d . . .
N12 N 0.3970(2) 0.81867(9) 0.13373(14) 0.0182(4) Uani 1 1 d . . .
O30 O 0.1124(2) 0.7500 0.2002(2) 0.0215(5) Uani 1 2 d S . .
N11 N 0.47610(19) 0.80830(9) 0.05329(13) 0.0182(4) Uani 1 1 d . . .
C1 C 0.5634(3) 0.7500 0.0497(2) 0.0181(7) Uani 1 2 d S . .
H1A H 0.6281 0.7500 0.1061 0.022 Uiso 1 2 calc SR . .
H1B H 0.6185 0.7500 -0.0115 0.022 Uiso 1 2 calc SR . .
C13 C 0.3301(2) 0.87442(12) 0.1171(2) 0.0255(6) Uani 1 1 d . A .
H13 H 0.2654 0.8936 0.1611 0.031 Uiso 1 1 calc R . .
C14 C 0.3670(3) 0.90133(13) 0.0268(2) 0.0311(6) Uani 1 1 d . . .
C26' C 0.3681(3) 0.99483(13) -0.0939(2) 0.0289(6) Uani 0.431(9) 1 d P A 2
H26' H 0.4561 0.9811 -0.1173 0.035 Uiso 0.431(9) 1 calc PR A 2
C15 C 0.4606(2) 0.85731(12) -0.01184(18) 0.0260(5) Uani 1 1 d . A .
H15 H 0.5060 0.8610 -0.0734 0.031 Uiso 1 1 calc R . .
C27A C 0.1376(16) 1.1455(7) -0.1175(10) 0.025(2) Uani 0.569(9) 1 d P A 1
C24 C 0.2032(13) 1.0853(6) -0.0763(8) 0.0231(16) Uani 0.569(9) 1 d P A 1
H31 H 0.088(3) 0.7806(13) 0.176(2) 0.035 Uiso 1 1 d . . .
O29A O 0.0154(9) 1.1581(4) -0.0900(7) 0.079(3) Uani 0.569(9) 1 d P A 1
O29B O -0.0054(8) 1.1368(4) -0.1407(7) 0.046(2) Uani 0.431(9) 1 d P A 2
C22A C 0.2238(11) 1.0030(5) 0.0474(8) 0.071(3) Uani 0.569(9) 1 d P A 1
H22A H 0.1960 0.9871 0.1099 0.086 Uiso 0.569(9) 1 calc PR A 1
C22B C 0.1740(11) 0.9781(6) 0.0020(11) 0.062(4) Uani 0.431(9) 1 d P A 2
H22B H 0.1237 0.9537 0.0495 0.075 Uiso 0.431(9) 1 calc PR A 2
C23B C 0.1146(10) 1.0351(6) -0.0363(11) 0.065(4) Uani 0.431(9) 1 d P A 2
H23B H 0.0244 1.0485 -0.0169 0.078 Uiso 0.431(9) 1 calc PR A 2
C23A C 0.1665(10) 1.0599(4) 0.0106(7) 0.064(3) Uani 0.569(9) 1 d P A 1
H23A H 0.0983 1.0821 0.0484 0.077 Uiso 0.569(9) 1 calc PR A 1
C21A C 0.3218(18) 0.9689(8) -0.0066(14) 0.025(2) Uani 0.569(9) 1 d P A 1
C27B C 0.116(2) 1.1350(9) -0.1419(13) 0.022(3) Uani 0.431(9) 1 d P A 2
C21B C 0.301(2) 0.9561(10) -0.0257(18) 0.024(3) Uani 0.431(9) 1 d P A 2
C5 C 0.1918(18) 1.0724(8) -0.1047(11) 0.0231(16) Uani 0.431(9) 1 d P A 2
C25' C 0.3125(3) 1.05320(12) -0.12973(19) 0.0286(6) Uani 0.431(9) 1 d P A 2
H25' H 0.3654 1.0793 -0.1738 0.034 Uiso 0.431(9) 1 calc PR A 2
C26 C 0.3681(3) 0.99483(13) -0.0939(2) 0.0289(6) Uani 0.569(9) 1 d P A 1
H26 H 0.4384 0.9728 -0.1299 0.035 Uiso 0.569(9) 1 calc PR A 1
C25 C 0.3125(3) 1.05320(12) -0.12973(19) 0.0286(6) Uani 0.569(9) 1 d P A 1
H25 H 0.3464 1.0717 -0.1890 0.034 Uiso 0.569(9) 1 calc PR A 1
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
O28 Cu1 O28 95.33(9) 2_575 7_656
O28 Cu1 N12 88.25(7) 2_575 .
O28 Cu1 N12 174.29(8) 7_656 .
O28 Cu1 N12 174.29(8) 2_575 8_575
O28 Cu1 N12 88.25(7) 7_656 8_575
N12 Cu1 N12 87.84(11) . 8_575
O28 Cu1 O30 81.95(7) 2_575 .
O28 Cu1 O30 81.95(7) 7_656 .
N12 Cu1 O30 94.19(7) . .
N12 Cu1 O30 94.19(7) 8_575 .
C27A O28 C27B 20.0(8) . .
C27A O28 Cu1 132.5(7) . 2_574
C27B O28 Cu1 123.3(8) . 2_574
C13 N12 N11 105.71(19) . .
C13 N12 Cu1 127.26(16) . .
N11 N12 Cu1 124.81(14) . .
Cu1 O30 H31 114(2) . .
C15 N11 N12 110.92(18) . .
C15 N11 C1 130.3(2) . .
N12 N11 C1 118.76(19) . .
N11 C1 N11 109.0(2) . 8_575
N11 C1 H1A 109.9 . .
N11 C1 H1A 109.9 8_575 .
N11 C1 H1B 109.9 . .
N11 C1 H1B 109.9 8_575 .
H1A C1 H1B 108.3 . .
N12 C13 C14 111.2(2) . .
N12 C13 H13 124.4 . .
C14 C13 H13 124.4 . .
C15 C14 C13 104.5(2) . .
C15 C14 C21B 126.3(10) . .
C13 C14 C21B 128.0(10) . .
C15 C14 C21A 131.7(8) . .
C13 C14 C21A 123.3(8) . .
C21B C14 C21A 16.1(8) . .
C21B C26' C25' 122.7(11) . .
C21B C26' H26' 118.6 . .
C25' C26' H26' 118.6 . .
N11 C15 C14 107.6(2) . .
N11 C15 H15 126.2 . .
C14 C15 H15 126.2 . .
O28 C27A O29A 124.1(13) . .
O28 C27A C24 119.0(13) . .
O29A C27A C24 116.9(13) . .
C23A C24 C27A 122.5(11) . .
C23A C22A C21A 120.1(11) . .
C23A C22A H22A 119.9 . .
C21A C22A H22A 119.9 . .
C21B C22B C23B 122.9(14) . .
C21B C22B H22B 118.6 . .
C23B C22B H22B 118.6 . .
C22B C23B C5 118.3(11) . .
C22B C23B H23B 120.8 . .
C5 C23B H23B 120.8 . .
C24 C23A C22A 122.6(8) . .
C24 C23A H23A 118.7 . .
C22A C23A H23A 118.7 . .
C22A C21A C14 119.5(14) . .
O29B C27B O28 128.6(16) . .
O29B C27B C5 119.7(16) . .
O28 C27B C5 111.6(16) . .
C22B C21B C26' 115.0(19) . .
C22B C21B C14 120.6(19) . .
C26' C21B C14 123.6(17) . .
C25' C5 C23B 119.6(14) . .
C25' C5 C27B 126.6(16) . .
C23B C5 C27B 113.8(15) . .
C5 C25' C26' 121.4(9) . .
C5 C25' H25' 119.3 . .
C26' C25' H25' 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O28 1.9556(15) 2_575
Cu1 O28 1.9556(15) 7_656
Cu1 N12 2.0129(19) .
Cu1 N12 2.0129(19) 8_575
Cu1 O30 2.363(2) .
O28 C27A 1.223(17) .
O28 C27B 1.31(2) .
O28 Cu1 1.9556(15) 2_574
N12 C13 1.324(3) .
N12 N11 1.353(3) .
O30 H31 0.74(3) .
N11 C15 1.343(3) .
N11 C1 1.456(2) .
C1 N11 1.456(2) 8_575
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C13 C14 1.394(4) .
C13 H13 0.9500 .
C14 C15 1.377(4) .
C14 C21B 1.47(3) .
C14 C21A 1.511(19) .
C26' C21B 1.38(2) .
C26' C25' 1.391(3) .
C26' H26' 0.9500 .
C15 H15 0.9500 .
C27A O29A 1.266(19) .
C27A C24 1.49(2) .
C24 C23A 1.340(14) .
O29B C27B 1.17(2) .
C22A C23A 1.377(11) .
C22A C21A 1.39(2) .
C22A H22A 0.9500 .
C22B C21B 1.36(3) .
C22B C23B 1.394(15) .
C22B H22B 0.9500 .
C23B C5 1.41(2) .
C23B H23B 0.9500 .
C23A H23A 0.9500 .
C27B C5 1.55(3) .
C5 C25' 1.276(17) .
C25' H25' 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O28 Cu1 N12 C13 -36.3(2) 2_575 .
O28 Cu1 N12 C13 92.7(7) 7_656 .
N12 Cu1 N12 C13 139.50(19) 8_575 .
O30 Cu1 N12 C13 45.5(2) . .
O28 Cu1 N12 N11 163.07(18) 2_575 .
O28 Cu1 N12 N11 -67.9(8) 7_656 .
N12 Cu1 N12 N11 -21.1(2) 8_575 .
O30 Cu1 N12 N11 -115.14(17) . .
C13 N12 N11 C15 1.0(3) . .
Cu1 N12 N11 C15 165.05(16) . .
C13 N12 N11 C1 179.8(2) . .
Cu1 N12 N11 C1 -16.2(3) . .
C15 N11 C1 N11 -119.1(3) . 8_575
N12 N11 C1 N11 62.4(3) . 8_575
N11 N12 C13 C14 -1.1(3) . .
Cu1 N12 C13 C14 -164.65(18) . .
N12 C13 C14 C15 0.8(3) . .
N12 C13 C14 C21B 169.0(7) . .
N12 C13 C14 C21A -172.0(6) . .
N12 N11 C15 C14 -0.5(3) . .
C1 N11 C15 C14 -179.1(2) . .
C13 C14 C15 N11 -0.2(3) . .
C21B C14 C15 N11 -168.6(7) . .
C21A C14 C15 N11 171.7(6) . .
C27B O28 C27A O29A -82(5) . .
Cu1 O28 C27A O29A -11.8(14) 2_574 .
C27B O28 C27A C24 97(5) . .
Cu1 O28 C27A C24 166.9(4) 2_574 .
O28 C27A C24 C23A 154.8(9) . .
O29A C27A C24 C23A -26.3(14) . .
C21B C22B C23B C5 -2(2) . .
C27A C24 C23A C22A 177.8(9) . .
C21A C22A C23A C24 -1.1(16) . .
C23A C22A C21A C14 -170.4(9) . .
C15 C14 C21A C22A -180.0(8) . .
C13 C14 C21A C22A -9.4(12) . .
C21B C14 C21A C22A 103(6) . .
C27A O28 C27B O29B 108(6) . .
Cu1 O28 C27B O29B -16(2) 2_574 .
C27A O28 C27B C5 -76(4) . .
Cu1 O28 C27B C5 160.4(6) 2_574 .
C23B C22B C21B C26' 1(2) . .
C23B C22B C21B C14 171.2(11) . .
C25' C26' C21B C22B 1.8(16) . .
C25' C26' C21B C14 -168.2(8) . .
C15 C14 C21B C22B 152.0(11) . .
C13 C14 C21B C22B -13.8(16) . .
C21A C14 C21B C22B -93(6) . .
C15 C14 C21B C26' -38.6(15) . .
C13 C14 C21B C26' 155.7(10) . .
C21A C14 C21B C26' 77(5) . .
C22B C23B C5 C25' 0.3(17) . .
C22B C23B C5 C27B -179.8(10) . .
O29B C27B C5 C25' 154.8(13) . .
O28 C27B C5 C25' -22.0(16) . .
O29B C27B C5 C23B -25.1(18) . .
O28 C27B C5 C23B 158.0(11) . .
C23B C5 C25' C26' 2.4(12) . .
C27B C5 C25' C26' -177.6(8) . .
C21B C26' C25' C5 -3.6(10) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 0.250 0.250 491 53 ' '
2 -0.039 0.750 0.750 491 53 ' '
