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#$Date: 2015-06-07 01:47:41 +0300 (Sun, 07 Jun 2015) $
#$Revision: 138601 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/49/7034943.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_7034943
loop_
_publ_author_name
'Wu, Wei-Ping'
'Li, Zhi-Sen'
'Liu, Bo'
'Liu, Ping'
'Xi, Zheng-Ping'
'Wang, Yao-Yu'
_publ_section_title
;
 Double-step CO2 sorption and guest-induced
 single-crystal-to-single-crystal transformation in a flexible porous
 framework.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10141
_journal_page_last               10145
_journal_paper_doi               10.1039/c5dt00460h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C36 H44 Cu2 N6 O13'
_chemical_formula_weight         895.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-03-17 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                99.393(8)
_cell_angle_beta                 104.513(8)
_cell_angle_gamma                102.434(8)
_cell_formula_units_Z            1
_cell_length_a                   8.976(4)
_cell_length_b                   10.699(5)
_cell_length_c                   11.570(6)
_cell_measurement_reflns_used    4278
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.866
_cell_measurement_theta_min      3.136
_cell_volume                     1022.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15767
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.366
_diffrn_reflns_theta_min         1.868
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3762
_reflns_number_total             5055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt00460h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7034943--7034944.cif.'
_cod_original_cell_volume        1022.3(9)
_cod_database_code               7034943
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.809
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 1.0000 1.0000 0.0000 0.03068(18) Uani 1 2 d S . P
Cu2 Cu 0.5000 0.0000 0.5000 0.02342(17) Uani 1 2 d S . P
O3 O 0.9568(3) 0.7556(2) 0.5181(2) 0.0315(5) Uani 1 1 d . . .
O5 O 0.7326(4) 0.2016(3) 0.6465(3) 0.0440(7) Uani 1 1 d . . .
O4 O 0.5603(3) 0.1714(2) 0.4629(2) 0.0304(5) Uani 1 1 d . . .
O1 O 0.9680(3) 0.9452(3) 0.1471(2) 0.0402(6) Uani 1 1 d . . .
O2 O 0.8078(4) 1.0784(3) 0.1488(3) 0.0571(9) Uani 1 1 d . . .
C3 C 0.9142(4) 0.8684(3) 0.3557(3) 0.0267(7) Uani 1 1 d . . .
H3 H 0.9960 0.8435 0.3302 0.032 Uiso 1 1 calc R U .
C11 C 0.8833(4) 0.4613(3) 0.6346(3) 0.0318(7) Uani 1 1 d . . .
H11 H 0.9319 0.4300 0.7005 0.038 Uiso 1 1 calc R U .
C12 C 0.9506(4) 0.5874(3) 0.6249(3) 0.0298(7) Uani 1 1 d . . .
H12 H 1.0435 0.6403 0.6836 0.036 Uiso 1 1 calc R U .
N1 N 0.6702(3) 0.9437(3) 0.4337(3) 0.0252(6) Uani 1 1 d . . .
C7 C 0.8771(4) 0.6329(3) 0.5263(3) 0.0249(6) Uani 1 1 d . . .
C2 C 0.8324(4) 0.9492(3) 0.2976(3) 0.0264(7) Uani 1 1 d . . .
C10 C 0.7449(4) 0.3815(3) 0.5477(3) 0.0284(7) Uani 1 1 d . . .
C4 C 0.8700(4) 0.8267(3) 0.4521(3) 0.0248(6) Uani 1 1 d . . .
C5 C 0.7473(4) 0.8639(3) 0.4875(3) 0.0266(7) Uani 1 1 d . . .
H5 H 0.7168 0.8327 0.5509 0.032 Uiso 1 1 calc R U .
C13 C 0.6768(4) 0.2428(3) 0.5551(3) 0.0300(7) Uani 1 1 d . . .
C6 C 0.7136(4) 0.9861(3) 0.3405(3) 0.0262(7) Uani 1 1 d . . .
H6 H 0.6619 1.0423 0.3035 0.031 Uiso 1 1 calc R U .
C8 C 0.7378(5) 0.5569(3) 0.4398(4) 0.0384(9) Uani 1 1 d . . .
H8 H 0.6878 0.5897 0.3754 0.046 Uiso 1 1 calc R U .
C9 C 0.6728(4) 0.4298(3) 0.4502(4) 0.0379(9) Uani 1 1 d . . .
H9 H 0.5801 0.3770 0.3912 0.045 Uiso 1 1 calc R U .
C1 C 0.8697(4) 0.9968(4) 0.1893(3) 0.0360(8) Uani 1 1 d . . .
N2 N 1.2163(4) 1.1178(4) 0.0993(3) 0.0456(9) Uani 1 1 d . . .
C14 C 1.2040(7) 1.2321(5) 0.1834(5) 0.0642(14) Uani 1 1 d . . .
H14A H 1.1462 1.2021 0.2375 0.096 Uiso 1 1 calc R U .
H14B H 1.1486 1.2835 0.1367 0.096 Uiso 1 1 calc R U .
H14C H 1.3092 1.2851 0.2307 0.096 Uiso 1 1 calc R U .
C15 C 1.3240(6) 1.0486(6) 0.1640(5) 0.0693(15) Uani 1 1 d . . .
H15A H 1.4272 1.1090 0.2046 0.104 Uiso 1 1 calc R U .
H15B H 1.3341 0.9781 0.1060 0.104 Uiso 1 1 calc R U .
H15C H 1.2809 1.0135 0.2236 0.104 Uiso 1 1 calc R U .
N3 N 0.3492(6) 0.6673(6) 0.0470(6) 0.0948(19) Uani 1 1 d . . .
O6 O 0.5832(7) 0.7319(7) 0.0169(7) 0.147(3) Uani 1 1 d . . .
C18 C 0.4314(12) 0.7226(10) -0.0115(11) 0.135(4) Uani 1 1 d . . .
H027 H 0.3841 0.7572 -0.0755 0.162 Uiso 1 1 calc R U .
C17 C 0.4092(14) 0.6082(11) 0.1453(10) 0.143(4) Uani 1 1 d . . .
H17A H 0.5222 0.6211 0.1604 0.214 Uiso 1 1 calc R U .
H17B H 0.3570 0.5157 0.1232 0.214 Uiso 1 1 calc R U .
H17C H 0.3885 0.6482 0.2181 0.214 Uiso 1 1 calc R U .
C16 C 0.1833(9) 0.6740(11) 0.0324(10) 0.142(4) Uani 1 1 d . . .
H16A H 0.1749 0.7163 0.1094 0.213 Uiso 1 1 calc R U .
H16B H 0.1130 0.5866 0.0061 0.213 Uiso 1 1 calc R U .
H16C H 0.1540 0.7233 -0.0278 0.213 Uiso 1 1 calc R U .
H2A H 1.269(6) 1.149(5) 0.051(5) 0.062(15) Uiso 1 1 d . . .
O1W O 0.140(2) 0.3599(13) 0.8969(11) 0.165(6) Uani 0.5 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'
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
O1 Cu1 O1 180.00(16) . 2_775
O1 Cu1 N2 89.95(14) . 2_775
O1 Cu1 N2 90.05(14) 2_775 2_775
O1 Cu1 N2 90.05(14) . .
O1 Cu1 N2 89.95(14) 2_775 .
N2 Cu1 N2 180.0(2) 2_775 .
O4 Cu2 O4 180.0 . 2_656
O4 Cu2 N1 89.64(10) . 2_666
O4 Cu2 N1 90.36(10) 2_656 2_666
O4 Cu2 N1 90.36(10) . 1_545
O4 Cu2 N1 89.64(10) 2_656 1_545
N1 Cu2 N1 180.00(14) 2_666 1_545
C7 O3 C4 118.4(3) . .
C13 O4 Cu2 106.5(2) . .
C1 O1 Cu1 113.1(2) . .
C4 C3 C2 118.1(3) . .
C10 C11 C12 121.2(3) . .
C7 C12 C11 118.9(3) . .
C5 N1 C6 118.1(3) . .
C5 N1 Cu2 118.8(2) . 1_565
C6 N1 Cu2 123.1(2) . 1_565
C8 C7 O3 123.0(3) . .
C8 C7 C12 121.4(3) . .
O3 C7 C12 115.6(3) . .
C6 C2 C3 118.9(3) . .
C6 C2 C1 119.3(3) . .
C3 C2 C1 121.8(3) . .
C11 C10 C9 118.8(3) . .
C11 C10 C13 121.0(3) . .
C9 C10 C13 120.1(3) . .
C5 C4 C3 119.9(3) . .
C5 C4 O3 120.3(3) . .
C3 C4 O3 119.6(3) . .
N1 C5 C4 122.3(3) . .
O5 C13 O4 122.9(3) . .
O5 C13 C10 120.7(3) . .
O4 C13 C10 116.4(3) . .
N1 C6 C2 122.6(3) . .
C7 C8 C9 119.0(3) . .
C10 C9 C8 120.8(3) . .
O2 C1 O1 125.3(3) . .
O2 C1 C2 119.9(3) . .
O1 C1 C2 114.7(3) . .
C15 N2 C14 111.7(4) . .
C15 N2 Cu1 113.8(3) . .
C14 N2 Cu1 111.6(3) . .
C18 N3 C17 124.6(8) . .
C18 N3 C16 121.6(8) . .
C17 N3 C16 113.2(7) . .
N3 C18 O6 119.8(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.954(3) .
Cu1 O1 1.954(3) 2_775
Cu1 N2 2.008(4) 2_775
Cu1 N2 2.008(4) .
Cu2 O4 1.946(2) .
Cu2 O4 1.946(2) 2_656
Cu2 N1 2.029(3) 2_666
Cu2 N1 2.029(3) 1_545
O3 C7 1.383(4) .
O3 C4 1.385(4) .
O5 C13 1.242(4) .
O4 C13 1.284(4) .
O1 C1 1.288(5) .
O2 C1 1.227(5) .
C3 C4 1.382(4) .
C3 C2 1.396(5) .
C11 C10 1.386(5) .
C11 C12 1.389(5) .
C12 C7 1.384(5) .
N1 C5 1.345(4) .
N1 C6 1.346(4) .
N1 Cu2 2.029(3) 1_565
C7 C8 1.377(5) .
C2 C6 1.386(4) .
C2 C1 1.513(4) .
C10 C9 1.389(5) .
C10 C13 1.503(4) .
C4 C5 1.379(4) .
C8 C9 1.397(5) .
N2 C15 1.473(6) .
N2 C14 1.476(6) .
N3 C18 1.243(9) .
N3 C17 1.434(10) .
N3 C16 1.474(9) .
O6 C18 1.297(11) .
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
C10 C11 C12 C7 0.0(5) .
C4 O3 C7 C8 25.4(5) .
C4 O3 C7 C12 -157.6(3) .
C11 C12 C7 C8 1.3(5) .
C11 C12 C7 O3 -175.7(3) .
C4 C3 C2 C6 1.4(5) .
C4 C3 C2 C1 -178.4(3) .
C12 C11 C10 C9 -0.5(5) .
C12 C11 C10 C13 177.0(3) .
C2 C3 C4 C5 0.6(5) .
C2 C3 C4 O3 -174.8(3) .
C7 O3 C4 C5 61.5(4) .
C7 O3 C4 C3 -123.2(3) .
C6 N1 C5 C4 1.2(5) .
Cu2 N1 C5 C4 -176.6(2) 1_565
C3 C4 C5 N1 -2.0(5) .
O3 C4 C5 N1 173.3(3) .
Cu2 O4 C13 O5 0.1(4) .
Cu2 O4 C13 C10 180.0(2) .
C11 C10 C13 O5 8.2(5) .
C9 C10 C13 O5 -174.4(4) .
C11 C10 C13 O4 -171.6(3) .
C9 C10 C13 O4 5.8(5) .
C5 N1 C6 C2 0.9(5) .
Cu2 N1 C6 C2 178.6(2) 1_565
C3 C2 C6 N1 -2.2(5) .
C1 C2 C6 N1 177.6(3) .
O3 C7 C8 C9 174.8(3) .
C12 C7 C8 C9 -2.1(6) .
C11 C10 C9 C8 -0.3(6) .
C13 C10 C9 C8 -177.8(4) .
C7 C8 C9 C10 1.5(6) .
Cu1 O1 C1 O2 -4.4(5) .
Cu1 O1 C1 C2 175.7(2) .
C6 C2 C1 O2 7.9(5) .
C3 C2 C1 O2 -172.3(4) .
C6 C2 C1 O1 -172.2(3) .
C3 C2 C1 O1 7.6(5) .
C17 N3 C18 O6 -1.4(16) .
C16 N3 C18 O6 169.5(10) .
