#------------------------------------------------------------------------------
#$Date: 2019-11-17 10:30:17 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229354 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/75/7047521.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_7047521
loop_
_publ_author_name
'Pandey, Saurabh'
'Kumar, Pramod'
'Gupta, Rajeev'
_publ_section_title
;
 Polymerization led selective detection and removal of Zn²⁺ and
 Cd²⁺ ions: isolation of Zn- and Cd-MOFs and reversibility
 studies.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14686
_journal_page_last               14695
_journal_paper_doi               10.1039/c8dt01956h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(C66 H46 Cd2 N10 O12), 12[H2O]'
_chemical_formula_sum            'C33 H47 Cd N5 O18'
_chemical_formula_weight         914.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-08 deposited with the CCDC.
2018-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.699(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.987(7)
_cell_length_b                   12.635(3)
_cell_length_c                   19.051(5)
_cell_measurement_reflns_used    103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.65
_cell_volume                     4549(2)
_computing_cell_refinement       'Bruker Kappa Apex'
_computing_data_collection       'Bruker Kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2016/4)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18193
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         2.242
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.104
_refine_diff_density_min         -2.280
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.1031
_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)+(0.1131P)²+73.6342P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2545
_refine_ls_wR_factor_ref         0.2608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3382
_reflns_number_total             4023
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01956h2.cif
_cod_data_source_block           Cd(II)-L2
_cod_depositor_comments
'Adding full bibliography for 7047521--7047523.cif.'
_cod_database_code               7047521
_shelx_shelxl_version_number     2016/4
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C8(H8), C9(H9), C13(H13), C6(H6), C7(H7), C16(H16), C12(H12),
 C2(H2), C1(H1)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 512 electrons were
found in a volume of 2196Å^3 in 1 void.
This is consistent with the presence of
12[H2O] per formula unit
which account for 480.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Cd1 Cd 0.500000 0.48454(7) 0.750000 0.0339(3) Uani 1 2 d S TU P
N1 N 0.4583(3) 0.4223(6) 0.6113(5) 0.0430(16) Uani 1 1 d . U .
O3 O 0.0748(3) 0.8821(6) 0.2706(4) 0.0532(17) Uani 1 1 d . U .
O2 O 0.1271(4) 1.0333(6) 0.2889(5) 0.0623(19) Uani 1 1 d . U .
N2 N 0.500000 0.3059(8) 0.750000 0.046(2) Uani 1 2 d S TU P
O1 O 0.4460(4) 0.2699(6) 0.5377(5) 0.065(2) Uani 1 1 d . U .
C14 C 0.1899(5) 0.8780(8) 0.2967(6) 0.046(2) Uani 1 1 d . U .
C17 C 0.1260(4) 0.9346(9) 0.2863(5) 0.044(2) Uani 1 1 d . U .
N3 N 0.3957(4) 0.6381(8) 0.4128(6) 0.057(2) Uani 1 1 d . U .
C4 C 0.4575(5) 0.3213(8) 0.6006(7) 0.050(2) Uani 1 1 d . U .
C15 C 0.1839(5) 0.7785(9) 0.2697(7) 0.060(3) Uani 1 1 d . U .
H15 H 0.139724 0.742844 0.242533 0.072 Uiso 1 1 calc R . .
C3 C 0.4818(5) 0.2550(8) 0.6804(7) 0.053(2) Uani 1 1 d . U .
C5 C 0.4372(4) 0.4907(8) 0.5427(6) 0.0467(19) Uani 1 1 d . U .
C10 C 0.3731(6) 0.7164(11) 0.3462(8) 0.073(4) Uani 1 1 d . U .
H10A H 0.363076 0.680824 0.294087 0.088 Uiso 1 1 calc R . .
H10B H 0.411919 0.767734 0.364973 0.088 Uiso 1 1 calc R . .
C8 C 0.4313(5) 0.6710(9) 0.4954(7) 0.057(2) Uani 1 1 d . U .
H8 H 0.440414 0.744283 0.508322 0.068 Uiso 1 1 calc R . .
C11 C 0.3068(5) 0.7760(10) 0.3251(7) 0.061(3) Uani 1 1 d . U .
C9 C 0.4544(5) 0.5987(8) 0.5609(7) 0.051(2) Uani 1 1 d . U .
H9 H 0.481984 0.622124 0.618488 0.061 Uiso 1 1 calc R . .
C13 C 0.2535(5) 0.9312(10) 0.3335(8) 0.067(3) Uani 1 1 d . U .
H13 H 0.256381 1.003994 0.347685 0.081 Uiso 1 1 calc R . .
C6 C 0.3992(6) 0.4636(9) 0.4552(7) 0.063(3) Uani 1 1 d . U .
H6 H 0.386729 0.391777 0.438744 0.075 Uiso 1 1 calc R . .
C7 C 0.3805(6) 0.5365(11) 0.3952(8) 0.070(3) Uani 1 1 d . U .
H7 H 0.355145 0.514442 0.337333 0.084 Uiso 1 1 calc R . .
C16 C 0.2425(6) 0.7270(11) 0.2813(8) 0.071(3) Uani 1 1 d . U .
H16 H 0.237637 0.657940 0.258808 0.085 Uiso 1 1 calc R . .
C12 C 0.3133(5) 0.8783(10) 0.3500(9) 0.071(3) Uani 1 1 d . U .
H12 H 0.357702 0.913304 0.378034 0.086 Uiso 1 1 calc R . .
C2 C 0.4818(8) 0.1453(9) 0.6787(10) 0.082(4) Uani 1 1 d . U .
H2 H 0.469288 0.108921 0.628245 0.098 Uiso 1 1 calc R . .
C1 C 0.500000 0.0897(14) 0.750000 0.099(7) Uani 1 2 d S TU P
H1 H 0.499999 0.014521 0.749999 0.119 Uiso 1 2 calc RS T 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'
Cd Cd -0.8075 1.2024 '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
N1 Cd1 N1 141.3(4) 2_656 .
N1 Cd1 O2 88.7(2) . 7_566
N1 Cd1 O2 88.0(2) . 8_566
N1 Cd1 O2 88.0(2) 2_656 7_566
N1 Cd1 O2 88.7(2) 2_656 8_566
N1 Cd1 C17 95.9(2) . 8_566
N1 Cd1 C17 98.2(2) . 7_566
N1 Cd1 C17 95.9(2) 2_656 7_566
N1 Cd1 C17 98.2(2) 2_656 8_566
O3 Cd1 N1 102.9(3) 8_566 .
O3 Cd1 N1 105.5(2) 7_566 .
O3 Cd1 N1 102.9(3) 7_566 2_656
O3 Cd1 N1 105.5(2) 8_566 2_656
O3 Cd1 O3 84.5(4) 8_566 7_566
O3 Cd1 O2 52.8(2) 7_566 7_566
O3 Cd1 O2 137.2(3) 7_566 8_566
O3 Cd1 O2 137.2(3) 8_566 7_566
O3 Cd1 O2 52.8(2) 8_566 8_566
O3 Cd1 C17 26.1(3) 7_566 7_566
O3 Cd1 C17 26.1(3) 8_566 8_566
O3 Cd1 C17 110.5(3) 7_566 8_566
O3 Cd1 C17 110.5(3) 8_566 7_566
O2 Cd1 O2 170.0(3) 7_566 8_566
O2 Cd1 C17 26.7(3) 7_566 7_566
O2 Cd1 C17 163.3(3) 7_566 8_566
O2 Cd1 C17 26.7(3) 8_566 8_566
O2 Cd1 C17 163.3(3) 8_566 7_566
N2 Cd1 N1 70.65(19) . .
N2 Cd1 N1 70.64(19) . 2_656
N2 Cd1 O3 137.75(18) . 8_566
N2 Cd1 O3 137.75(18) . 7_566
N2 Cd1 O2 84.99(17) . 7_566
N2 Cd1 O2 84.99(17) . 8_566
N2 Cd1 C17 111.7(2) . 7_566
N2 Cd1 C17 111.7(2) . 8_566
C17 Cd1 C17 136.6(5) 8_566 7_566
C4 N1 Cd1 117.6(7) . .
C4 N1 C5 119.7(9) . .
C5 N1 Cd1 122.6(6) . .
C17 O3 Cd1 99.6(6) . 7_566
C17 O2 Cd1 84.6(5) . 7_566
C3 N2 Cd1 119.4(6) . .
C3 N2 Cd1 119.4(6) 2_656 .
C3 N2 C3 121.3(12) 2_656 .
C15 C14 C17 120.4(9) . .
C15 C14 C13 120.1(9) . .
C13 C14 C17 119.5(10) . .
O3 C17 Cd1 54.4(4) . 7_566
O3 C17 O2 123.0(8) . .
O3 C17 C14 119.3(9) . .
O2 C17 Cd1 68.6(5) . 7_566
O2 C17 C14 117.5(9) . .
C14 C17 Cd1 171.9(7) . 7_566
C8 N3 C10 118.9(11) . .
C7 N3 C10 121.9(11) . .
C7 N3 C8 119.2(10) . .
N1 C4 C3 114.7(9) . .
O1 C4 N1 129.8(10) . .
O1 C4 C3 115.1(9) . .
C14 C15 H15 120.0 . .
C14 C15 C16 119.9(11) . .
C16 C15 H15 120.0 . .
N2 C3 C4 117.5(8) . .
N2 C3 C2 120.6(11) . .
C2 C3 C4 121.8(11) . .
N1 C5 C9 117.9(9) . .
N1 C5 C6 127.1(10) . .
C9 C5 C6 115.0(10) . .
N3 C10 H10A 109.3 . .
N3 C10 H10B 109.3 . .
N3 C10 C11 111.7(8) . .
H10A C10 H10B 107.9 . .
C11 C10 H10A 109.3 . .
C11 C10 H10B 109.3 . .
N3 C8 H8 119.7 . .
N3 C8 C9 120.6(11) . .
C9 C8 H8 119.7 . .
C16 C11 C10 120.5(12) . .
C12 C11 C10 118.7(11) . .
C12 C11 C16 120.9(9) . .
C5 C9 H9 119.7 . .
C8 C9 C5 120.6(10) . .
C8 C9 H9 119.7 . .
C14 C13 H13 119.9 . .
C14 C13 C12 120.2(11) . .
C12 C13 H13 119.9 . .
C5 C6 H6 119.2 . .
C7 C6 C5 121.6(12) . .
C7 C6 H6 119.2 . .
N3 C7 C6 122.9(12) . .
N3 C7 H7 118.5 . .
C6 C7 H7 118.5 . .
C15 C16 H16 120.1 . .
C11 C16 C15 119.8(12) . .
C11 C16 H16 120.1 . .
C11 C12 C13 118.7(11) . .
C11 C12 H12 120.7 . .
C13 C12 H12 120.7 . .
C3 C2 H2 120.2 . .
C1 C2 C3 119.7(13) . .
C1 C2 H2 120.2 . .
C2 C1 C2 118.2(16) . 2_656
C2 C1 H1 120.9 . .
C2 C1 H1 120.9 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N1 2.373(8) 2_656
Cd1 N1 2.373(8) .
Cd1 O3 2.277(6) 7_566
Cd1 O3 2.277(6) 8_566
Cd1 O2 2.584(7) 8_566
Cd1 O2 2.584(7) 7_566
Cd1 N2 2.258(10) .
Cd1 C17 2.762(8) 7_566
Cd1 C17 2.762(8) 8_566
N1 C4 1.291(12) .
N1 C5 1.403(13) .
O3 Cd1 2.277(6) 7_566
O3 C17 1.230(12) .
O2 Cd1 2.584(7) 7_566
O2 C17 1.248(12) .
N2 C3 1.310(11) 2_656
N2 C3 1.310(11) .
O1 C4 1.252(12) .
C14 C17 1.542(11) .
C14 C15 1.335(15) .
C14 C13 1.383(15) .
C17 Cd1 2.762(8) 7_566
N3 C10 1.452(14) .
N3 C8 1.361(14) .
N3 C7 1.323(16) .
C4 C3 1.535(15) .
C15 H15 0.9500 .
C15 C16 1.396(14) .
C3 C2 1.387(15) .
C5 C9 1.407(14) .
C5 C6 1.415(15) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C10 C11 1.536(12) .
C8 H8 0.9500 .
C8 C9 1.385(14) .
C11 C16 1.363(17) .
C11 C12 1.356(18) .
C9 H9 0.9500 .
C13 H13 0.9500 .
C13 C12 1.395(14) .
C6 H6 0.9500 .
C6 C7 1.333(17) .
C7 H7 0.9500 .
C16 H16 0.9500 .
C12 H12 0.9500 .
C2 H2 0.9500 .
C2 C1 1.366(16) .
C1 C2 1.366(16) 2_656
C1 H1 0.9500 .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.414 -0.694 -0.450 2196.5 512.2 '6 water'
