#------------------------------------------------------------------------------
#$Date: 2016-06-01 06:24:36 +0300 (Wed, 01 Jun 2016) $
#$Revision: 183193 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/53/7225385.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_7225385
loop_
_publ_author_name
'Linder-Patton, Oliver M.'
'Bloch, Witold M.'
'Coghlan, Campbell J.'
'Sumida, Kenji'
'Kitagawa, Susumu'
'Furukawa, Shuhei'
'Doonan, Christian J.'
'Sumby, Christopher J.'
_publ_section_title
;
 Particle size effects in the kinetic trapping of a structurally-locked
 form of a flexible MOF
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4172
_journal_paper_doi               10.1039/C6CE00082G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C30 H34 Cu N4 O8'
_chemical_formula_weight         642.15
_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
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2536(2)
_cell_length_b                   19.8774(4)
_cell_length_c                   14.8763(7)
_cell_measurement_reflns_used    4840
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0053
_cell_measurement_theta_min      2.4596
_cell_volume                     3032.01(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 0.987
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details
;
  1 omega   -9.00   92.00   1.0000  144.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   37.0000  -30.0000 101

  2 omega  -13.00   15.00   1.0000  144.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463  -37.0000 -180.0000 28

  3 omega   71.00   96.00   1.0000  144.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463 -160.0000  -71.0000 25

  4 omega   -9.00   92.00   1.0000  144.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8463   37.0000 -150.0000 101

;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14195
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84318
_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    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0454
_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)+(0.0672P)²+2.8510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                2888
_reflns_number_total             3623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00082g2.cif
_cod_data_source_block           Cu-bcppm-H2O-acetone
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7225385
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 0.68572(4) 0.2500 0.25668(3) 0.01308(14) Uani 1 2 d S
O29 O 0.77327(17) -0.17877(8) 0.67123(12) 0.0178(4) Uani 1 1 d .
O1 O 0.9037(3) 0.2500 0.2875(2) 0.0196(6) Uani 1 2 d S
O28 O 0.97466(19) -0.14590(11) 0.63369(17) 0.0393(6) Uani 1 1 d .
N11 N 0.6398(2) 0.17974(9) 0.34854(14) 0.0157(4) Uani 1 1 d .
N12 N 0.55867(18) 0.19038(10) 0.41961(14) 0.0157(4) Uani 1 1 d .
C15 C 0.7022(2) 0.12233(11) 0.36691(18) 0.0179(5) Uani 1 1 d .
H15 H 0.7665 0.1025 0.3293 0.021 Uiso 1 1 calc R
C1 C 0.4770(3) 0.2500 0.4203(3) 0.0166(7) Uani 1 2 d S
H1A H 0.4195 0.2500 0.3668 0.020 Uiso 1 2 calc SR
H1B H 0.4214 0.2500 0.4747 0.020 Uiso 1 2 calc SR
C25 C 0.6789(2) -0.05341(12) 0.60605(19) 0.0213(5) Uani 1 1 d .
H25 H 0.6288 -0.0732 0.6528 0.026 Uiso 1 1 calc R
C24 C 0.7973(2) -0.08241(12) 0.58048(19) 0.0213(5) Uani 1 1 d .
C14 C 0.6601(2) 0.09524(12) 0.44922(18) 0.0181(5) Uani 1 1 d .
C13 C 0.5680(2) 0.14108(12) 0.48090(18) 0.0186(5) Uani 1 1 d .
H13 H 0.5206 0.1380 0.5356 0.022 Uiso 1 1 calc R
C21 C 0.7046(2) 0.03310(12) 0.49308(19) 0.0208(5) Uani 1 1 d .
C26 C 0.6346(2) 0.00407(12) 0.56337(19) 0.0210(5) Uani 1 1 d .
H26 H 0.5550 0.0241 0.5823 0.025 Uiso 1 1 calc R
C27 C 0.8541(3) -0.14034(12) 0.63224(18) 0.0209(5) Uani 1 1 d .
C22 C 0.8201(3) 0.00201(14) 0.4650(2) 0.0318(7) Uani 1 1 d .
H22 H 0.8673 0.0197 0.4153 0.038 Uiso 1 1 calc R
C23 C 0.8657(3) -0.05451(14) 0.5095(2) 0.0314(7) Uani 1 1 d .
H23 H 0.9454 -0.0745 0.4909 0.038 Uiso 1 1 calc R
O43 O 0.3952(5) 0.1350(3) 0.6557(3) 0.1237(18) Uani 1 1 d .
C42 C 0.2297(9) 0.1411(7) 0.7640(5) 0.213(6) Uani 1 1 d .
H42A H 0.2155 0.1858 0.7380 0.319 Uiso 1 1 calc R
H42B H 0.2422 0.1453 0.8291 0.319 Uiso 1 1 calc R
H42C H 0.1537 0.1126 0.7519 0.319 Uiso 1 1 calc R
C40 C 0.3483(6) 0.1101(4) 0.7228(4) 0.0878(18) Uani 1 1 d .
C41 C 0.3986(11) 0.0487(4) 0.7658(5) 0.159(4) Uani 1 1 d .
H41A H 0.3374 0.0116 0.7557 0.238 Uiso 1 1 calc R
H41B H 0.4083 0.0564 0.8306 0.238 Uiso 1 1 calc R
H41C H 0.4836 0.0372 0.7399 0.238 Uiso 1 1 calc R
H7 H 0.922(3) 0.2783(18) 0.311(3) 0.050(13) Uiso 1 1 d .
C52 C 1.1183(6) 0.2500 0.5490(4) 0.0605(15) Uani 1 2 d S
H52A H 1.1381 0.2080 0.5806 0.091 Uiso 0.50 1 calc PR
H52B H 1.1825 0.2843 0.5658 0.091 Uiso 0.50 1 calc PR
H52C H 1.1220 0.2424 0.4840 0.091 Uiso 0.50 1 calc PR
C51 C 0.8708(7) 0.2500 0.5270(5) 0.078(2) Uani 1 2 d S
H51A H 0.8751 0.2010 0.5204 0.117 Uiso 0.50 1 calc PR
H51B H 0.8675 0.2710 0.4675 0.117 Uiso 0.50 1 calc PR
H51C H 0.7924 0.2621 0.5610 0.117 Uiso 0.50 1 calc PR
C50 C 0.9848(9) 0.2734(4) 0.5745(5) 0.062(2) Uani 0.50 1 d P
O53 O 0.9712(8) 0.3179(5) 0.6291(6) 0.134(4) Uani 0.50 1 d P
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
O29 Cu1 O29 93.20(10) 2_654 7_765
O29 Cu1 N11 177.37(7) 2_654 8_565
O29 Cu1 N11 89.38(8) 7_765 8_565
O29 Cu1 N11 89.38(8) 2_654 .
O29 Cu1 N11 177.37(7) 7_765 .
N11 Cu1 N11 88.03(11) 8_565 .
O29 Cu1 O1 85.39(8) 2_654 .
O29 Cu1 O1 85.39(8) 7_765 .
N11 Cu1 O1 95.33(8) 8_565 .
N11 Cu1 O1 95.33(8) . .
C27 O29 Cu1 126.55(16) . 2_655
Cu1 O1 H7 112(3) . .
C15 N11 N12 105.5(2) . .
C15 N11 Cu1 128.33(18) . .
N12 N11 Cu1 124.26(14) . .
C13 N12 N11 111.75(19) . .
C13 N12 C1 129.3(2) . .
N11 N12 C1 119.0(2) . .
N11 C15 C14 111.0(2) . .
N11 C15 H15 124.5 . .
C14 C15 H15 124.5 . .
N12 C1 N12 109.5(3) 8_565 .
N12 C1 H1A 109.8 8_565 .
N12 C1 H1A 109.8 . .
N12 C1 H1B 109.8 8_565 .
N12 C1 H1B 109.8 . .
H1A C1 H1B 108.2 . .
C26 C25 C24 120.1(2) . .
C26 C25 H25 120.0 . .
C24 C25 H25 120.0 . .
C23 C24 C25 118.9(2) . .
C23 C24 C27 120.1(2) . .
C25 C24 C27 120.9(2) . .
C13 C14 C15 104.6(2) . .
C13 C14 C21 127.5(2) . .
C15 C14 C21 127.8(2) . .
N12 C13 C14 107.2(2) . .
N12 C13 H13 126.4 . .
C14 C13 H13 126.4 . .
C26 C21 C22 118.5(2) . .
C26 C21 C14 121.4(2) . .
C22 C21 C14 120.1(2) . .
C25 C26 C21 121.1(2) . .
C25 C26 H26 119.4 . .
C21 C26 H26 119.4 . .
O28 C27 O29 126.1(2) . .
O28 C27 C24 117.6(2) . .
O29 C27 C24 116.3(2) . .
C23 C22 C21 120.0(3) . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C24 C23 C22 121.3(3) . .
C24 C23 H23 119.4 . .
C22 C23 H23 119.4 . .
C40 C42 H42A 109.5 . .
C40 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C40 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
O43 C40 C41 123.8(7) . .
O43 C40 C42 119.5(7) . .
C41 C40 C42 116.7(6) . .
C40 C41 H41A 109.5 . .
C40 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C40 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C50 C52 H52A 109.5 . .
C50 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C50 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
C50 C51 H51A 109.5 . .
C50 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
C50 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
O53 C50 C51 118.1(9) . .
O53 C50 C52 120.3(8) . .
C51 C50 C52 121.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O29 1.9486(16) 2_654
Cu1 O29 1.9487(16) 7_765
Cu1 N11 2.010(2) 8_565
Cu1 N11 2.010(2) .
Cu1 O1 2.282(3) .
O29 C27 1.267(3) .
O29 Cu1 1.9486(16) 2_655
O1 H7 0.69(3) .
O28 C27 1.242(3) .
N11 C15 1.337(3) .
N11 N12 1.362(3) .
N12 C13 1.342(3) .
N12 C1 1.451(3) .
C15 C14 1.405(3) .
C15 H15 0.9500 .
C1 N12 1.451(3) 8_565
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C25 C26 1.384(3) .
C25 C24 1.397(4) .
C25 H25 0.9500 .
C24 C23 1.384(4) .
C24 C27 1.502(3) .
C14 C13 1.395(3) .
C14 C21 1.470(3) .
C13 H13 0.9500 .
C21 C26 1.394(4) .
C21 C22 1.400(4) .
C26 H26 0.9500 .
C22 C23 1.385(4) .
C22 H22 0.9500 .
C23 H23 0.9500 .
O43 C40 1.214(6) .
C42 C40 1.495(10) .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C40 C41 1.471(10) .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C52 C50 1.494(11) .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
C51 C50 1.443(11) .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
C50 O53 1.209(10) .
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
O29 Cu1 N11 C15 41.9(2) 2_654 .
O29 Cu1 N11 C15 -149.1(16) 7_765 .
N11 Cu1 N11 C15 -138.56(18) 8_565 .
O1 Cu1 N11 C15 -43.4(2) . .
O29 Cu1 N11 N12 -156.38(19) 2_654 .
O29 Cu1 N11 N12 12.6(18) 7_765 .
N11 Cu1 N11 N12 23.1(2) 8_565 .
O1 Cu1 N11 N12 118.32(18) . .
C15 N11 N12 C13 -0.6(3) . .
Cu1 N11 N12 C13 -165.79(16) . .
C15 N11 N12 C1 179.5(2) . .
Cu1 N11 N12 C1 14.3(3) . .
N12 N11 C15 C14 0.9(3) . .
Cu1 N11 C15 C14 165.26(17) . .
C13 N12 C1 N12 118.5(3) . 8_565
N11 N12 C1 N12 -61.5(4) . 8_565
C26 C25 C24 C23 -2.9(4) . .
C26 C25 C24 C27 173.5(2) . .
N11 C15 C14 C13 -0.8(3) . .
N11 C15 C14 C21 -179.9(2) . .
N11 N12 C13 C14 0.1(3) . .
C1 N12 C13 C14 -180.0(2) . .
C15 C14 C13 N12 0.4(3) . .
C21 C14 C13 N12 179.5(2) . .
C13 C14 C21 C26 16.2(4) . .
C15 C14 C21 C26 -164.9(3) . .
C13 C14 C21 C22 -163.3(3) . .
C15 C14 C21 C22 15.5(4) . .
C24 C25 C26 C21 1.6(4) . .
C22 C21 C26 C25 1.4(4) . .
C14 C21 C26 C25 -178.2(2) . .
Cu1 O29 C27 O28 8.6(4) 2_655 .
Cu1 O29 C27 C24 -170.74(17) 2_655 .
C23 C24 C27 O28 26.2(4) . .
C25 C24 C27 O28 -150.2(3) . .
C23 C24 C27 O29 -154.5(3) . .
C25 C24 C27 O29 29.2(4) . .
C26 C21 C22 C23 -3.0(5) . .
C14 C21 C22 C23 176.5(3) . .
C25 C24 C23 C22 1.3(5) . .
C27 C24 C23 C22 -175.1(3) . .
C21 C22 C23 C24 1.7(5) . .
