#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:14:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180253 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/39/7113967.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_7113967
loop_
_publ_author_name
'Prem Lama'
'Raj Kumar Das'
'Vincent J. Smith'
'Leonard J. Barbour'
_publ_section_title
;
 A combined stretching-tilting mechanism produces negative, zero and
 positive linear thermal expansion in a semi-flexible Cd(II)-MOF
;
_journal_name_full               Chem.Commun.
_journal_page_first              6464
_journal_paper_doi               10.1039/C4CC02634A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C53 H58 Cd2 N7 O19'
_chemical_formula_sum            'C53 H58 Cd2 N7 O19'
_chemical_formula_weight         1321.86
_chemical_name_common            1
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.159(1)
_cell_angle_beta                 76.657(1)
_cell_angle_gamma                88.223(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2817(10)
_cell_length_b                   12.0978(12)
_cell_length_c                   12.6236(13)
_cell_measurement_reflns_used    571
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      1.72
_cell_volume                     1476.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       12
_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            13056
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.9154
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             673
_exptl_crystal_size_max          0.611
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0292P)²+0.9171P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                5415
_reflns_number_total             5828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02634a3.cif
_cod_data_source_block           180
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113967
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.602443(14) 0.981918(12) 0.628000(13) 0.01660(6) Uani 1 1 d . . .
O1 O 0.43164(15) 1.10188(14) 0.65056(14) 0.0247(4) Uani 1 1 d . . .
O2 O 0.35736(15) 0.98089(12) 0.57074(13) 0.0211(3) Uani 1 1 d . . .
O3 O -0.15292(16) 0.96204(13) 0.64294(15) 0.0265(4) Uani 1 1 d . . .
O4 O -0.24595(15) 1.12931(13) 0.59977(14) 0.0240(4) Uani 1 1 d . . .
O5 O -0.02774(19) 1.45949(17) 0.6753(2) 0.0537(6) Uani 1 1 d . . .
O6 O 0.19296(17) 1.47761(14) 0.60373(16) 0.0307(4) Uani 1 1 d . . .
H6A H 0.1797 1.5466 0.6030 0.037 Uiso 1 1 calc R . .
O7 O 1.1033(6) -0.0895(5) 0.8621(5) 0.0750(16) Uani 0.50 1 d P . .
N1 N 0.59882(18) 0.79017(15) 0.63459(16) 0.0196(4) Uani 1 1 d . . .
N2 N 0.4474(2) 0.08013(17) 1.17079(17) 0.0263(4) Uani 1 1 d . . .
N3 N 1.0000 0.0000 1.0000 0.0580(11) Uani 1 2 d S . .
C1 C 0.3428(2) 1.06659(18) 0.61255(18) 0.0187(4) Uani 1 1 d . . .
C2 C 0.2141(2) 1.12902(18) 0.61789(18) 0.0175(4) Uani 1 1 d . . .
C3 C 0.0996(2) 1.07364(18) 0.61335(18) 0.0176(4) Uani 1 1 d . . .
H3 H 0.1039 0.9975 0.6054 0.021 Uiso 1 1 calc R . .
C4 C -0.0212(2) 1.12957(19) 0.62042(19) 0.0195(5) Uani 1 1 d . . .
C5 C -0.1476(2) 1.06887(19) 0.62076(19) 0.0200(5) Uani 1 1 d . . .
C6 C -0.0264(2) 1.24166(19) 0.6299(2) 0.0221(5) Uani 1 1 d . . .
H6 H -0.1087 1.2800 0.6350 0.027 Uiso 1 1 calc R . .
C7 C 0.0889(2) 1.29814(19) 0.6320(2) 0.0219(5) Uani 1 1 d . . .
C8 C 0.0775(2) 1.4196(2) 0.6392(2) 0.0281(5) Uani 1 1 d . . .
C9 C 0.2086(2) 1.24123(18) 0.62725(18) 0.0188(4) Uani 1 1 d . . .
H9 H 0.2868 1.2789 0.6304 0.023 Uiso 1 1 calc R . .
C10 C 0.4931(2) 0.73632(19) 0.6225(2) 0.0245(5) Uani 1 1 d . . .
H10 H 0.4169 0.7794 0.6094 0.029 Uiso 1 1 calc R . .
C11 C 0.4906(2) 0.6204(2) 0.6282(2) 0.0270(5) Uani 1 1 d . . .
H11 H 0.4138 0.5859 0.6185 0.032 Uiso 1 1 calc R . .
C12 C 0.5989(2) 0.55475(18) 0.64788(19) 0.0217(5) Uani 1 1 d . . .
C13 C 0.7091(2) 0.6110(2) 0.6588(2) 0.0251(5) Uani 1 1 d . . .
H13 H 0.7867 0.5698 0.6711 0.030 Uiso 1 1 calc R . .
C14 C 0.7054(2) 0.72618(19) 0.6517(2) 0.0245(5) Uani 1 1 d . . .
H14 H 0.7821 0.7627 0.6592 0.029 Uiso 1 1 calc R . .
C15 C 0.5952(3) 0.42714(19) 0.6640(2) 0.0262(5) Uani 1 1 d . . .
H15A H 0.6830 0.4028 0.6268 0.031 Uiso 1 1 calc R . .
H15B H 0.5265 0.4060 0.6286 0.031 Uiso 1 1 calc R . .
C16 C 0.5631(3) 0.3661(2) 0.7889(2) 0.0323(6) Uani 1 1 d . . .
H16A H 0.4766 0.3929 0.8257 0.039 Uiso 1 1 calc R . .
H16B H 0.6328 0.3875 0.8232 0.039 Uiso 1 1 calc R . .
C17 C 0.5549(3) 0.2358(2) 0.8125(2) 0.0322(6) Uani 1 1 d . . .
H17A H 0.4869 0.2139 0.7768 0.039 Uiso 1 1 calc R . .
H17B H 0.6423 0.2081 0.7786 0.039 Uiso 1 1 calc R . .
C18 C 0.5187(3) 0.17979(19) 0.9369(2) 0.0285(6) Uani 1 1 d . . .
C19 C 0.3908(3) 0.1869(2) 1.0005(2) 0.0375(6) Uani 1 1 d . . .
H19 H 0.3244 0.2263 0.9652 0.045 Uiso 1 1 calc R . .
C20 C 0.3597(3) 0.1368(2) 1.1152(2) 0.0375(6) Uani 1 1 d . . .
H20 H 0.2712 0.1430 1.1566 0.045 Uiso 1 1 calc R . .
C21 C 0.5708(3) 0.0733(2) 1.1093(2) 0.0319(6) Uani 1 1 d . . .
H21 H 0.6353 0.0332 1.1465 0.038 Uiso 1 1 calc R . .
C22 C 0.6096(3) 0.1216(2) 0.9943(2) 0.0319(6) Uani 1 1 d . . .
H22 H 0.6989 0.1147 0.9550 0.038 Uiso 1 1 calc R . .
C23 C 1.0647(13) 0.0062(10) 0.8943(7) 0.105(4) Uani 0.50 1 d P . .
C24 C 0.9715(9) 0.0945(8) 1.0474(8) 0.071(2) Uani 0.50 1 d P . .
C25 C 0.9276(10) -0.1098(7) 1.0770(7) 0.078(3) Uani 0.50 1 d P . .
O8A O 0.1175(6) 0.3418(5) 1.0598(4) 0.072(2) Uani 0.493(7) 1 d P A 1
N4A N 0.1711(14) 0.5253(14) 0.9773(14) 0.054(3) Uani 0.493(7) 1 d P A 1
C26A C 0.1380(11) 0.4375(9) 1.0661(9) 0.061(2) Uani 0.493(7) 1 d P A 1
H26A H 0.1299 0.4501 1.1386 0.073 Uiso 0.493(7) 1 calc PR A 1
C27A C 0.179(2) 0.508(2) 0.8680(15) 0.129(10) Uani 0.493(7) 1 d P A 1
H27A H 0.2311 0.4398 0.8605 0.194 Uiso 0.493(7) 1 calc PR A 1
H27B H 0.2237 0.5749 0.8103 0.194 Uiso 0.493(7) 1 calc PR A 1
H27C H 0.0892 0.4974 0.8582 0.194 Uiso 0.493(7) 1 calc PR A 1
C28A C 0.1888(19) 0.6389(11) 0.9902(17) 0.144(7) Uani 0.493(7) 1 d P A 1
H28A H 0.1663 0.6371 1.0704 0.217 Uiso 0.493(7) 1 calc PR A 1
H28B H 0.1301 0.6914 0.9515 0.217 Uiso 0.493(7) 1 calc PR A 1
H28C H 0.2821 0.6651 0.9574 0.217 Uiso 0.493(7) 1 calc PR A 1
O8B O 0.1430(8) 0.3582(5) 0.9009(6) 0.095(3) Uani 0.507(7) 1 d P A 2
N4B N 0.2105(16) 0.5116(15) 0.9492(13) 0.054(3) Uani 0.507(7) 1 d P A 2
C26B C 0.1722(18) 0.4649(18) 0.8782(17) 0.090(6) Uani 0.507(7) 1 d P A 2
H26B H 0.1658 0.5121 0.8069 0.107 Uiso 0.507(7) 1 calc PR A 2
C27B C 0.2151(12) 0.4492(9) 1.0628(8) 0.067(3) Uani 0.507(7) 1 d P A 2
H27D H 0.1706 0.3741 1.0809 0.100 Uiso 0.507(7) 1 calc PR A 2
H27E H 0.1694 0.4922 1.1161 0.100 Uiso 0.507(7) 1 calc PR A 2
H27F H 0.3085 0.4393 1.0683 0.100 Uiso 0.507(7) 1 calc PR A 2
C28B C 0.2489(18) 0.6335(11) 0.9173(10) 0.101(5) Uani 0.507(7) 1 d P A 2
H28D H 0.2358 0.6688 0.8416 0.151 Uiso 0.507(7) 1 calc PR A 2
H28E H 0.3432 0.6420 0.9180 0.151 Uiso 0.507(7) 1 calc PR A 2
H28F H 0.1934 0.6713 0.9712 0.151 Uiso 0.507(7) 1 calc PR A 2
O1W O 0.1845(2) 1.69173(15) 0.59772(18) 0.0329(4) Uani 1 1 d D . .
O2W O 0.0061(2) 0.79004(18) 0.73741(19) 0.0464(5) Uani 1 1 d D . .
H1W2 H -0.038(3) 0.842(2) 0.709(2) 0.036(8) Uiso 1 1 d D . .
H2W1 H 0.202(3) 1.740(2) 0.5375(17) 0.035(8) Uiso 1 1 d D . .
H1W1 H 0.124(3) 1.721(3) 0.638(3) 0.054(11) Uiso 1 1 d D . .
H2W2 H -0.0533 0.7546 0.7940 0.050 Uiso 1 1 d D . .
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'
Cd Cd -0.8075 1.2024 '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 Cd1 N1 129.84(6) . .
O1 Cd1 O4 90.37(6) . 1_655
N1 Cd1 O4 139.79(6) . 1_655
O1 Cd1 O2 96.96(6) . 2_676
N1 Cd1 O2 87.57(6) . 2_676
O4 Cd1 O2 87.26(5) 1_655 2_676
O1 Cd1 N2 85.98(7) . 2_667
N1 Cd1 N2 85.28(7) . 2_667
O4 Cd1 N2 99.63(6) 1_655 2_667
O2 Cd1 N2 172.52(6) 2_676 2_667
O1 Cd1 O3 140.16(5) . 1_655
N1 Cd1 O3 87.78(6) . 1_655
O4 Cd1 O3 53.50(5) 1_655 1_655
O2 Cd1 O3 97.29(5) 2_676 1_655
N2 Cd1 O3 84.63(6) 2_667 1_655
C1 O1 Cd1 105.44(14) . .
C1 O2 Cd1 117.23(13) . 2_676
C5 O3 Cd1 86.33(13) . 1_455
C5 O4 Cd1 97.84(13) . 1_455
C24 O7 C23 59.3(6) 2_757 .
C10 N1 C14 116.76(19) . .
C10 N1 Cd1 122.85(15) . .
C14 N1 Cd1 120.39(14) . .
C20 N2 C21 116.3(2) . .
C20 N2 Cd1 121.92(17) . 2_667
C21 N2 Cd1 121.18(17) . 2_667
C23 N3 C23 180.0(11) . 2_757
C23 N3 C24 125.1(6) . .
C23 N3 C24 54.9(6) 2_757 .
C23 N3 C24 54.9(6) . 2_757
C23 N3 C24 125.1(6) 2_757 2_757
C24 N3 C24 179.999(3) . 2_757
C23 N3 C25 58.3(6) . 2_757
C23 N3 C25 121.7(6) 2_757 2_757
C24 N3 C25 67.6(5) . 2_757
C24 N3 C25 112.4(5) 2_757 2_757
C23 N3 C25 121.7(6) . .
C23 N3 C25 58.3(6) 2_757 .
C24 N3 C25 112.4(5) . .
C24 N3 C25 67.6(5) 2_757 .
C25 N3 C25 179.998(1) 2_757 .
O1 C1 O2 122.9(2) . .
O1 C1 C2 117.93(19) . .
O2 C1 C2 119.15(19) . .
C9 C2 C3 120.1(2) . .
C9 C2 C1 120.54(19) . .
C3 C2 C1 119.39(19) . .
C4 C3 C2 120.09(19) . .
C6 C4 C3 119.69(19) . .
C6 C4 C5 119.6(2) . .
C3 C4 C5 120.73(19) . .
O3 C5 O4 122.27(19) . .
O3 C5 C4 119.7(2) . .
O4 C5 C4 118.00(19) . .
C4 C6 C7 120.3(2) . .
C9 C7 C6 119.8(2) . .
C9 C7 C8 122.50(19) . .
C6 C7 C8 117.7(2) . .
O5 C8 O6 124.0(2) . .
O5 C8 C7 122.6(2) . .
O6 C8 C7 113.5(2) . .
C7 C9 C2 120.02(19) . .
N1 C10 C11 122.6(2) . .
C12 C11 C10 120.4(2) . .
C11 C12 C13 116.9(2) . .
C11 C12 C15 121.7(2) . .
C13 C12 C15 121.3(2) . .
C14 C13 C12 119.8(2) . .
N1 C14 C13 123.5(2) . .
C12 C15 C16 110.42(19) . .
C15 C16 C17 113.6(2) . .
C18 C17 C16 111.6(2) . .
C22 C18 C19 116.5(2) . .
C22 C18 C17 122.8(2) . .
C19 C18 C17 120.8(2) . .
C20 C19 C18 120.1(3) . .
N2 C20 C19 123.5(3) . .
N2 C21 C22 123.6(2) . .
C18 C22 C21 120.1(2) . .
C24 C23 N3 65.9(6) 2_757 .
C24 C23 O7 55.1(7) 2_757 .
N3 C23 O7 120.2(9) . .
C24 C23 C25 132.6(9) 2_757 2_757
N3 C23 C25 67.9(6) . 2_757
O7 C23 C25 160.0(12) . 2_757
O7 C24 C23 65.6(7) 2_757 2_757
O7 C24 N3 124.0(8) 2_757 .
C23 C24 N3 59.2(6) 2_757 .
O7 C24 C25 176.4(9) 2_757 2_757
C23 C24 C25 118.0(8) 2_757 2_757
N3 C24 C25 59.5(4) . 2_757
C23 C25 N3 53.9(5) 2_757 .
C23 C25 C24 106.2(6) 2_757 2_757
N3 C25 C24 52.9(4) . 2_757
C26A N4A C27A 118.8(16) . .
C26A N4A C28A 120.7(14) . .
C27A N4A C28A 120.3(17) . .
O8A C26A N4A 123.1(11) . .
C26B N4B C27B 123.4(17) . .
C26B N4B C28B 120.7(17) . .
C27B N4B C28B 116.0(13) . .
O8B C26B N4B 122.6(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O1 2.2570(16) .
Cd1 N1 2.3010(18) .
Cd1 O4 2.3080(15) 1_655
Cd1 O2 2.3711(16) 2_676
Cd1 N2 2.392(2) 2_667
Cd1 O3 2.5648(16) 1_655
O1 C1 1.256(3) .
O2 C1 1.269(3) .
O2 Cd1 2.3710(16) 2_676
O3 C5 1.250(3) .
O3 Cd1 2.5648(16) 1_455
O4 C5 1.267(3) .
O4 Cd1 2.3081(15) 1_455
O5 C8 1.210(3) .
O6 C8 1.322(3) .
O7 C24 1.209(10) 2_757
O7 C23 1.342(12) .
N1 C10 1.342(3) .
N1 C14 1.349(3) .
N2 C20 1.336(3) .
N2 C21 1.338(3) .
N2 Cd1 2.392(2) 2_667
N3 C23 1.331(8) .
N3 C23 1.331(8) 2_757
N3 C24 1.414(8) .
N3 C24 1.414(8) 2_757
N3 C25 1.527(7) 2_757
N3 C25 1.527(7) .
C1 C2 1.500(3) .
C2 C9 1.391(3) .
C2 C3 1.392(3) .
C3 C4 1.391(3) .
C4 C6 1.390(3) .
C4 C5 1.511(3) .
C6 C7 1.395(3) .
C7 C9 1.387(3) .
C7 C8 1.495(3) .
C10 C11 1.387(3) .
C11 C12 1.380(3) .
C12 C13 1.390(3) .
C12 C15 1.505(3) .
C13 C14 1.373(3) .
C15 C16 1.523(3) .
C16 C17 1.529(3) .
C17 C18 1.505(3) .
C18 C22 1.380(4) .
C18 C19 1.387(4) .
C19 C20 1.384(4) .
C21 C22 1.386(4) .
C23 C24 1.267(13) 2_757
C23 C25 1.401(13) 2_757
C24 O7 1.209(10) 2_757
C24 C23 1.267(13) 2_757
C24 C25 1.639(12) 2_757
C25 C23 1.401(13) 2_757
C25 C24 1.639(12) 2_757
O8A C26A 1.209(12) .
N4A C26A 1.32(2) .
N4A C27A 1.43(2) .
N4A C28A 1.45(2) .
O8B C26B 1.28(2) .
N4B C26B 1.31(2) .
N4B C27B 1.45(2) .
N4B C28B 1.47(2) .
