#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:14:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179473 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/70/4337039.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_4337039
loop_
_publ_author_name
'Dani Peri'
'Jim Ciston'
'Felipe Gándara'
'Yingbo Zhao'
'Omar M. Yaghi'
_publ_section_title
;
 Crystalline Fibers of Metal-Peptide Double Ladders
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13818
_journal_page_last               13820
_journal_paper_doi               10.1021/ic402435z
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C30 H30 Cd N5 O14'
_chemical_formula_sum            'C30 H30 Cd N5 O14'
_chemical_formula_weight         796.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 115.556(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.319(2)
_cell_length_b                   4.8688(5)
_cell_length_c                   20.288(2)
_cell_measurement_temperature    200(2)
_cell_volume                     1632.5(3)
_computing_data_collection       APEXII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1636
_diffrn_reflns_av_sigmaI/netI    0.1397
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20475
_diffrn_reflns_theta_full        66.01
_diffrn_reflns_theta_max         66.01
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    6.044
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       needle
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.613
_refine_diff_density_min         -2.444
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.034(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1285
_refine_ls_R_factor_gt           0.0946
_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)+(0.1214P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2327
_reflns_number_gt                4002
_reflns_number_total             5414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402435z_si_003.cif
_cod_data_source_block           MODL
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4337039
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
Cd1 Cd 0.72201(5) -0.0800(2) 0.37863(5) 0.0273(3) Uani 1 1 d .
O3 O 0.8383(5) -0.298(2) 0.4569(6) 0.040(3) Uani 1 1 d .
O5 O 0.3260(6) 0.144(2) 0.7217(6) 0.039(3) Uani 1 1 d .
O2 O 0.7980(6) 0.137(2) 0.3306(7) 0.045(3) Uani 1 1 d .
O1 O 0.6078(5) 0.168(2) 0.3024(6) 0.043(3) Uani 1 1 d .
O15 O 0.5882(8) -0.192(2) 0.8048(8) 0.039(3) Uani 1 1 d .
O14 O 0.9239(7) -0.150(2) 0.7477(7) 0.042(3) Uani 1 1 d .
C2 C 0.9676(7) 0.232(3) 0.6994(8) 0.025(3) Uani 1 1 d .
H2 H 0.9987 0.3915 0.7294 0.030 Uiso 1 1 calc R
C50 C 0.9123(8) 0.332(3) 0.6212(9) 0.038(4) Uani 1 1 d .
H50A H 0.8986 0.5288 0.6209 0.046 Uiso 1 1 calc R
H50B H 0.8617 0.2234 0.5994 0.046 Uiso 1 1 calc R
C4 C 0.8825(7) 0.220(3) 0.9494(8) 0.028(3) Uani 1 1 d U
C5 C 0.9021(7) 0.302(3) 0.8861(8) 0.034(4) Uani 1 1 d .
H5A H 0.8997 0.5048 0.8823 0.041 Uiso 1 1 calc R
H5B H 0.9586 0.2471 0.8989 0.041 Uiso 1 1 calc R
C6 C 0.9202(9) 0.362(4) 1.0137(9) 0.053(6) Uani 1 1 d U
H6 H 0.9549 0.5114 1.0166 0.063 Uiso 1 1 calc R
C8 C 0.8195(8) -0.057(5) 1.0071(9) 0.044(4) Uani 1 1 d U
H8 H 0.7840 -0.2036 1.0045 0.053 Uiso 1 1 calc R
O13 O 0.7521(6) 0.5522(19) 0.7788(7) 0.030(3) Uani 1 1 d .
O8 O 0.8731(7) 0.157(3) 1.1923(7) 0.052(3) Uani 1 1 d .
C12 C 0.8573(8) 0.083(3) 1.0703(9) 0.035(3) Uani 1 1 d U
N4 N 0.7065(6) 0.115(2) 0.7706(6) 0.022(3) Uani 1 1 d U
H4 H 0.7209 -0.0586 0.7767 0.026 Uiso 1 1 calc R
C15 C 0.5956(10) 0.054(3) 0.8013(11) 0.031(4) Uani 1 1 d .
N7 N 0.5845(7) 0.237(2) 0.8468(6) 0.024(3) Uani 1 1 d .
H7 H 0.5908 0.4132 0.8416 0.029 Uiso 1 1 calc R
C18 C 0.6208(7) 0.185(3) 0.7466(7) 0.020(3) Uani 1 1 d .
H18 H 0.6135 0.3890 0.7455 0.024 Uiso 1 1 calc R
O6 O 0.7410(5) 0.2795(19) 0.4526(6) 0.031(2) Uani 1 1 d .
O7 O 0.6624(5) 0.6487(19) 0.4302(5) 0.028(2) Uani 1 1 d .
C20 C 0.6877(6) 0.435(4) 0.4601(7) 0.024(3) Uani 1 1 d .
C21 C 0.3406(8) -0.027(3) 0.8390(9) 0.039(4) Uani 1 1 d .
H21A H 0.3295 0.0623 0.8776 0.047 Uiso 1 1 calc R
H21B H 0.3188 -0.2158 0.8327 0.047 Uiso 1 1 calc R
C24 C 0.5941(6) 0.465(3) 0.5208(7) 0.022(3) Uani 1 1 d U
H24 H 0.5702 0.6188 0.4902 0.026 Uiso 1 1 calc R
C22 C 0.6561(7) 0.325(2) 0.5142(8) 0.020(3) Uani 1 1 d U
C23 C 0.6902(7) 0.101(3) 0.5584(8) 0.025(3) Uani 1 1 d U
H23 H 0.7331 0.0050 0.5542 0.030 Uiso 1 1 calc R
O11 O 0.2293(6) 0.236(2) 0.7597(6) 0.046(3) Uani 1 1 d .
C26 C 0.5663(6) 0.385(3) 0.5714(7) 0.023(3) Uani 1 1 d U
H26 H 0.5250 0.4870 0.5768 0.027 Uiso 1 1 calc R
C27 C 0.5994(7) 0.156(3) 0.6140(8) 0.021(3) Uani 1 1 d U
C28 C 0.6634(7) 0.016(3) 0.6081(8) 0.024(3) Uani 1 1 d U
H28 H 0.6878 -0.1378 0.6386 0.029 Uiso 1 1 calc R
N3 N 0.4277(7) -0.043(3) 0.8642(7) 0.036(3) Uani 1 1 d .
H3 H 0.4512 -0.2042 0.8689 0.043 Uiso 1 1 calc R
C31 C 0.6096(11) 0.298(4) 0.9737(9) 0.058(5) Uani 1 1 d .
H31A H 0.5939 0.2321 1.0114 0.087 Uiso 1 1 calc R
H31B H 0.5979 0.4951 0.9657 0.087 Uiso 1 1 calc R
H31C H 0.6677 0.2676 0.9897 0.087 Uiso 1 1 calc R
C29 C 0.5627(8) 0.145(3) 0.9035(9) 0.033(4) Uani 1 1 d .
H29 H 0.5755 -0.0554 0.9124 0.039 Uiso 1 1 calc R
C34 C 0.8316(9) 0.009(3) 0.9443(10) 0.040(4) Uani 1 1 d U
H34 H 0.8050 -0.0917 0.9002 0.048 Uiso 1 1 calc R
C35 C 0.9083(10) 0.291(4) 1.0742(10) 0.052(5) Uani 1 1 d U
H35 H 0.9360 0.3884 1.1187 0.062 Uiso 1 1 calc R
C37 C 0.8426(8) 0.031(3) 1.1371(9) 0.030(4) Uani 1 1 d .
O9 O 0.7963(8) -0.180(3) 1.1288(7) 0.062(4) Uani 1 1 d .
C38 C 0.5705(7) 0.061(3) 0.6702(7) 0.023(3) Uani 1 1 d .
H38A H 0.5739 -0.1422 0.6737 0.028 Uiso 1 1 calc R
H38B H 0.5131 0.1131 0.6535 0.028 Uiso 1 1 calc R
C41 C 0.4721(8) 0.186(3) 0.8804(9) 0.037(4) Uani 1 1 d .
O12 O 0.4430(6) 0.416(3) 0.8711(7) 0.065(3) Uani 1 1 d .
C40 C 0.2957(9) 0.126(3) 0.7694(9) 0.034(4) Uani 1 1 d .
O19 O 1.0717(5) -0.043(3) 0.6044(5) 0.043(3) Uani 1 1 d .
C45 C 0.8491(7) 0.186(3) 0.8115(8) 0.022(3) Uani 1 1 d U
H45 H 0.8479 -0.0194 0.8140 0.026 Uiso 1 1 calc R
C47 C 0.7620(8) 0.302(3) 0.7832(10) 0.020(4) Uani 1 1 d U
N5 N 0.8836(6) 0.269(2) 0.7628(6) 0.027(3) Uani 1 1 d .
H5 H 0.8795 0.4420 0.7494 0.032 Uiso 1 1 calc R
C48 C 0.9213(8) 0.095(3) 0.7372(9) 0.024(4) Uani 1 1 d .
C51 C 0.9653(9) 0.283(3) 0.5804(9) 0.034(4) Uani 1 1 d .
H51A H 0.9329 0.2091 0.5308 0.041 Uiso 1 1 calc R
H51B H 0.9920 0.4551 0.5765 0.041 Uiso 1 1 calc R
N13 N 1.0230(6) 0.045(2) 0.6887(7) 0.029(3) Uani 1 1 d .
H13 H 1.0520 -0.0798 0.7208 0.034 Uiso 1 1 calc R
C55 C 1.0247(7) 0.082(3) 0.6265(9) 0.032(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O7 Cd1 O6 96.6(3) 1_545 .
O7 Cd1 O2 170.3(4) 1_545 .
O6 Cd1 O2 88.7(4) . .
O7 Cd1 O3 84.2(3) 1_545 .
O6 Cd1 O3 93.9(4) . .
O2 Cd1 O3 87.3(4) . .
O7 Cd1 O5 89.5(4) 1_545 2_646
O6 Cd1 O5 162.1(4) . 2_646
O2 Cd1 O5 87.8(4) . 2_646
O3 Cd1 O5 103.4(4) . 2_646
O7 Cd1 O1 97.8(3) 1_545 .
O6 Cd1 O1 82.9(4) . .
O2 Cd1 O1 90.9(4) . .
O3 Cd1 O1 176.3(4) . .
O5 Cd1 O1 79.7(4) 2_646 .
C40 O5 Cd1 125.3(9) . 2_656
N13 C2 C50 103.6(11) . .
N13 C2 C48 112.2(11) . .
C50 C2 C48 113.2(11) . .
N13 C2 H2 109.2 . .
C50 C2 H2 109.2 . .
C48 C2 H2 109.2 . .
C2 C50 C51 102.5(10) . .
C2 C50 H50A 111.3 . .
C51 C50 H50A 111.3 . .
C2 C50 H50B 111.3 . .
C51 C50 H50B 111.3 . .
H50A C50 H50B 109.2 . .
C34 C4 C6 120.0(15) . .
C34 C4 C5 122.4(15) . .
C6 C4 C5 117.6(13) . .
C45 C5 C4 117.5(11) . .
C45 C5 H5A 107.9 . .
C4 C5 H5A 107.9 . .
C45 C5 H5B 107.9 . .
C4 C5 H5B 107.9 . .
H5A C5 H5B 107.2 . .
C4 C6 C35 120.8(15) . .
C4 C6 H6 119.6 . .
C35 C6 H6 119.6 . .
C12 C8 C34 121.5(17) . .
C12 C8 H8 119.3 . .
C34 C8 H8 119.3 . .
C8 C12 C35 119.4(16) . .
C8 C12 C37 123.3(14) . .
C35 C12 C37 117.2(15) . .
C47 N4 C18 122.3(11) . .
C47 N4 H4 118.8 . .
C18 N4 H4 118.8 . .
O15 C15 N7 123.7(18) . .
O15 C15 C18 122.4(17) . .
N7 C15 C18 113.9(13) . .
C15 N7 C29 120.9(12) . .
C15 N7 H7 119.5 . .
C29 N7 H7 119.5 . .
N4 C18 C38 109.4(10) . .
N4 C18 C15 106.2(11) . .
C38 C18 C15 109.3(11) . .
N4 C18 H18 110.6 . .
C38 C18 H18 110.6 . .
C15 C18 H18 110.6 . .
C20 O6 Cd1 129.1(9) . .
C20 O7 Cd1 126.3(7) . 1_565
O7 C20 O6 126.6(12) . .
O7 C20 C22 118.9(11) . .
O6 C20 C22 114.5(14) . .
N3 C21 C40 115.8(12) . .
N3 C21 H21A 108.3 . .
C40 C21 H21A 108.3 . .
N3 C21 H21B 108.3 . .
C40 C21 H21B 108.3 . .
H21A C21 H21B 107.4 . .
C22 C24 C26 121.0(13) . .
C22 C24 H24 119.5 . .
C26 C24 H24 119.5 . .
C24 C22 C23 119.3(13) . .
C24 C22 C20 118.3(12) . .
C23 C22 C20 122.3(12) . .
C22 C23 C28 121.0(12) . .
C22 C23 H23 119.5 . .
C28 C23 H23 119.5 . .
C27 C26 C24 119.2(12) . .
C27 C26 H26 120.4 . .
C24 C26 H26 120.4 . .
C26 C27 C28 119.8(12) . .
C26 C27 C38 120.9(11) . .
C28 C27 C38 119.2(12) . .
C23 C28 C27 119.6(13) . .
C23 C28 H28 120.2 . .
C27 C28 H28 120.2 . .
C41 N3 C21 120.1(14) . .
C41 N3 H3 120.0 . .
C21 N3 H3 120.0 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N7 C29 C31 111.0(13) . .
N7 C29 C41 110.6(12) . .
C31 C29 C41 109.1(13) . .
N7 C29 H29 108.7 . .
C31 C29 H29 108.7 . .
C41 C29 H29 108.7 . .
C4 C34 C8 118.0(16) . .
C4 C34 H34 121.0 . .
C8 C34 H34 121.0 . .
C6 C35 C12 120.3(17) . .
C6 C35 H35 119.9 . .
C12 C35 H35 119.9 . .
O8 C37 O9 123.4(16) . .
O8 C37 C12 124.4(14) . .
O9 C37 C12 112.1(14) . .
C27 C38 C18 112.5(10) . .
C27 C38 H38A 109.1 . .
C18 C38 H38A 109.1 . .
C27 C38 H38B 109.1 . .
C18 C38 H38B 109.1 . .
H38A C38 H38B 107.8 . .
O12 C41 N3 123.4(13) . .
O12 C41 C29 120.6(14) . .
N3 C41 C29 115.6(13) . .
O11 C40 O5 122.8(14) . .
O11 C40 C21 117.3(13) . .
O5 C40 C21 119.9(13) . .
N5 C45 C5 107.4(10) . .
N5 C45 C47 109.2(11) . .
C5 C45 C47 110.2(11) . .
N5 C45 H45 110.0 . .
C5 C45 H45 110.0 . .
C47 C45 H45 110.0 . .
O13 C47 N4 126.7(14) . .
O13 C47 C45 119.0(13) . .
N4 C47 C45 114.1(12) . .
C48 N5 C45 122.9(11) . .
C48 N5 H5 118.5 . .
C45 N5 H5 118.5 . .
O14 C48 N5 123.2(14) . .
O14 C48 C2 122.2(13) . .
N5 C48 C2 114.4(11) . .
C55 C51 C50 103.2(12) . .
C55 C51 H51A 111.1 . .
C50 C51 H51A 111.1 . .
C55 C51 H51B 111.1 . .
C50 C51 H51B 111.1 . .
H51A C51 H51B 109.1 . .
C55 N13 C2 111.9(12) . .
C55 N13 H13 124.1 . .
C2 N13 H13 124.1 . .
O19 C55 N13 125.3(14) . .
O19 C55 C51 121.4(15) . .
N13 C55 C51 113.3(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O7 2.240(9) 1_545
Cd1 O6 2.233(10) .
Cd1 O2 2.274(9) .
Cd1 O3 2.294(10) .
Cd1 O5 2.275(11) 2_646
Cd1 O1 2.331(10) .
O5 C40 1.310(17) .
O5 Cd1 2.275(11) 2_656
O15 C15 1.212(15) .
O14 C48 1.208(18) .
C2 N13 1.449(16) .
C2 C50 1.55(2) .
C2 C48 1.522(18) .
C2 H2 1.0000 .
C50 C51 1.542(17) .
C50 H50A 0.9900 .
C50 H50B 0.9900 .
C4 C34 1.36(2) .
C4 C6 1.37(2) .
C4 C5 1.527(19) .
C5 C45 1.513(19) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C35 1.38(2) .
C6 H6 0.9500 .
C8 C12 1.35(2) .
C8 C34 1.42(2) .
C8 H8 0.9500 .
O13 C47 1.229(13) .
O8 C37 1.185(18) .
C12 C35 1.36(2) .
C12 C37 1.51(2) .
N4 C47 1.304(17) .
N4 C18 1.469(13) .
N4 H4 0.8800 .
C15 N7 1.36(2) .
C15 C18 1.52(2) .
N7 C29 1.443(16) .
N7 H7 0.8800 .
C18 C38 1.545(18) .
C18 H18 1.0000 .
O6 C20 1.297(17) .
O7 C20 1.19(2) .
O7 Cd1 2.240(9) 1_565
C20 C22 1.541(17) .
C21 N3 1.452(16) .
C21 C40 1.49(2) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C24 C22 1.380(16) .
C24 C26 1.383(17) .
C24 H24 0.9500 .
C22 C23 1.378(18) .
C23 C28 1.364(18) .
C23 H23 0.9500 .
O11 C40 1.265(17) .
C26 C27 1.38(2) .
C26 H26 0.9500 .
C27 C28 1.405(17) .
C27 C38 1.522(17) .
C28 H28 0.9500 .
N3 C41 1.33(2) .
N3 H3 0.8800 .
C31 C29 1.51(2) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C29 C41 1.531(18) .
C29 H29 1.0000 .
C34 H34 0.9500 .
C35 H35 0.9500 .
C37 O9 1.293(17) .
C38 H38A 0.9900 .
C38 H38B 0.9900 .
C41 O12 1.22(2) .
O19 C55 1.283(15) .
C45 N5 1.439(15) .
C45 C47 1.552(17) .
C45 H45 1.0000 .
N5 C48 1.332(17) .
N5 H5 0.8800 .
C51 C55 1.46(2) .
C51 H51A 0.9900 .
C51 H51B 0.9900 .
N13 C55 1.289(19) .
N13 H13 0.8800 .
