#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:51:24 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234938 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/96/4349641.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_4349641
loop_
_publ_author_name
'Margariti, A.'
'Rapti, S.'
'Katsenis, A. D.'
'Friščić, T.'
'Georgiou, Y.'
'Manos, M. J.'
'Papaefstathiou, G. S.'
_publ_section_title
;
 Cu2+ sorption from aqueous media by a recyclable Ca2+ framework
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              773
_journal_paper_doi               10.1039/C6QI00542J
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C34 H46 Ca N6 O14'
_chemical_formula_weight         802.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-30 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.283(3)
_cell_angle_beta                 105.014(2)
_cell_angle_gamma                92.062(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6342(19)
_cell_length_b                   10.239(2)
_cell_length_c                   10.592(2)
_cell_measurement_reflns_used    1514
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.72
_cell_measurement_theta_min      2.19
_cell_volume                     1008.0(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  APEXII,Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.870
_diffrn_reflns_theta_max         24.870
_diffrn_reflns_theta_min         1.991
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS (Bruker AXS Inc., Madison, Wisconsin, USA)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       Plates
_exptl_crystal_F_000             424
_exptl_crystal_preparation       ', ion exchange'
_exptl_crystal_recrystallization_method solvothermal
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3496
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0788
_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)+(0.1230P)²+0.6104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2250
_reflns_number_total             3496
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6qi00542j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4349641
_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.
;
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
C1 C 0.7461(4) 0.3118(5) 0.2862(4) 0.0535(12) Uani 1 1 d . . .
C2 C 0.5896(5) 0.2986(5) 0.2860(5) 0.0684(16) Uani 1 1 d . . .
C3 C 0.4879(4) 0.2087(4) 0.2097(4) 0.0418(10) Uani 1 1 d . . .
C4 C 0.3462(4) 0.2084(4) 0.2185(4) 0.0439(10) Uani 1 1 d . . .
H4 H 0.2781 0.1494 0.1668 0.053 Uiso 1 1 calc R U .
C5 C 0.3056(4) 0.2939(5) 0.3027(5) 0.0582(13) Uani 1 1 d . . .
C6 C 0.4049(6) 0.3824(9) 0.3767(9) 0.166(5) Uani 1 1 d . . .
H6 H 0.3777 0.4420 0.4324 0.200 Uiso 1 1 calc R U .
C7 C 0.5445(6) 0.3833(9) 0.3688(9) 0.163(5) Uani 1 1 d . . .
H7 H 0.6111 0.4430 0.4210 0.196 Uiso 1 1 calc R U .
C8 C 0.1565(4) 0.2948(4) 0.3195(4) 0.0474(11) Uani 1 1 d . . .
C9 C 0.4526(4) 0.0404(4) 0.0335(4) 0.0423(10) Uani 1 1 d . . .
C10 C 0.9526(7) 0.2557(9) 0.7022(10) 0.118(3) Uani 1 1 d . . .
C11 C 0.9105(10) 0.1097(7) 0.6177(8) 0.122(3) Uani 1 1 d . . .
H11A H 0.8909 0.1240 0.5257 0.183 Uiso 1 1 calc R U .
H11B H 0.9900 0.0534 0.6432 0.183 Uiso 1 1 calc R U .
H11C H 0.8271 0.0694 0.6368 0.183 Uiso 1 1 calc R U .
C12 C 0.9656(7) 0.1174(6) 0.8865(6) 0.0869(18) Uani 1 1 d . . .
H12A H 0.9974 0.1458 0.9768 0.130 Uiso 1 1 calc R U .
H12B H 0.8683 0.0827 0.8681 0.130 Uiso 1 1 calc R U .
H12C H 1.0266 0.0509 0.8692 0.130 Uiso 1 1 calc R U .
C13 C 1.0064(10) 0.3711(7) 0.8864(8) 0.126(3) Uani 1 1 d . . .
H13A H 1.0256 0.3578 0.9787 0.190 Uiso 1 1 calc R U .
H13B H 1.0885 0.4143 0.8677 0.190 Uiso 1 1 calc R U .
H13C H 0.9244 0.4242 0.8594 0.190 Uiso 1 1 calc R U .
C14 C 0.470(3) 0.174(2) 0.707(2) 0.220(11) Uani 1 1 d . . .
C15 C 0.337(2) 0.1224(17) 0.6474(17) 0.324(14) Uani 1 1 d . . .
H15A H 0.3446 0.0530 0.5873 0.487 Uiso 1 1 calc R U .
H15B H 0.2931 0.0885 0.7121 0.487 Uiso 1 1 calc R U .
H15C H 0.2796 0.1892 0.6007 0.487 Uiso 1 1 calc R U .
C16 C 0.6139(18) 0.3303(15) 0.8634(19) 0.254(9) Uani 1 1 d . . .
H16A H 0.5928 0.3977 0.9193 0.381 Uiso 1 1 calc R U .
H16B H 0.6730 0.2677 0.9158 0.381 Uiso 1 1 calc R U .
H16C H 0.6640 0.3684 0.8049 0.381 Uiso 1 1 calc R U .
C17 C 0.3547(18) 0.3162(17) 0.830(2) 0.310(13) Uani 1 1 d . . .
H17A H 0.3823 0.3868 0.8935 0.464 Uiso 1 1 calc R U .
H17B H 0.2874 0.3460 0.7533 0.464 Uiso 1 1 calc R U .
H17C H 0.3108 0.2455 0.8656 0.464 Uiso 1 1 calc R U .
N1 N 0.5341(4) 0.1212(3) 0.1265(4) 0.0454(9) Uani 1 1 d . . .
N2 N 0.9725(6) 0.2261(7) 0.8053(8) 0.120(3) Uani 1 1 d . . .
N3 N 0.4878(12) 0.2690(17) 0.7923(19) 0.204(7) Uani 1 1 d . . .
O1 O 0.8131(3) 0.4137(3) 0.3357(3) 0.0609(9) Uani 1 1 d . . .
O2 O 0.8007(3) 0.2194(3) 0.2369(3) 0.0685(11) Uani 1 1 d . . .
O3 O 0.3223(3) 0.0278(3) -0.0007(3) 0.0615(10) Uani 1 1 d . . .
O4 O 0.1317(3) 0.3524(3) 0.4116(3) 0.0590(9) Uani 1 1 d . . .
O5 O 0.0594(3) 0.2297(3) 0.2299(3) 0.0614(10) Uani 1 1 d D . .
O6 O 0.9549(4) 0.3484(4) 0.6362(4) 0.0823(12) Uani 1 1 d . . .
O7 O 0.6072(19) 0.164(2) 0.7015(18) 0.355(11) Uani 1 1 d . . .
Ca1 Ca 1.0000 0.5000 0.5000 0.0358(4) Uani 1 2 d S . P
H1 H 0.625(5) 0.119(4) 0.129(4) 0.043(11) Uiso 1 1 d . . .
H5 H -0.038(3) 0.229(6) 0.237(6) 0.11(2) 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'
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'
Ca Ca 0.2262 0.3064 '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'
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 C1 O2 124.2(4) . .
O1 C1 C2 117.0(4) . .
O2 C1 C2 118.8(4) . .
C7 C2 C3 117.8(4) . .
C7 C2 C1 116.5(4) . .
C3 C2 C1 125.7(4) . .
C4 C3 C2 119.6(3) . .
C4 C3 N1 122.5(3) . .
C2 C3 N1 117.9(3) . .
C5 C4 C3 120.8(4) . .
C5 C4 H4 119.6 . .
C3 C4 H4 119.6 . .
C6 C5 C4 119.6(4) . .
C6 C5 C8 117.3(4) . .
C4 C5 C8 123.1(4) . .
C5 C6 C7 120.0(5) . .
C5 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
C6 C7 C2 122.2(5) . .
C6 C7 H7 118.9 . .
C2 C7 H7 118.9 . .
O4 C8 O5 123.9(4) . .
O4 C8 C5 120.8(4) . .
O5 C8 C5 115.3(3) . .
O3 C9 N1 128.3(3) . .
O3 C9 C9 121.1(4) . 2_655
N1 C9 C9 110.7(4) . 2_655
N2 C10 O6 142.6(11) . .
N2 C10 C11 102.4(8) . .
O6 C10 C11 115.0(8) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N2 C12 H12A 109.5 . .
N2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N2 C13 H13A 109.5 . .
N2 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N2 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N3 C14 O7 99(2) . .
N3 C14 C15 121(3) . .
O7 C14 C15 140(3) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N3 C16 H16A 109.5 . .
N3 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
N3 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N3 C17 H17A 109.5 . .
N3 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N3 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C9 N1 C3 127.6(3) . .
C9 N1 H1 112(3) . .
C3 N1 H1 120(3) . .
C10 N2 C12 143.7(10) . .
C10 N2 C13 101.7(8) . .
C12 N2 C13 114.1(7) . .
C14 N3 C16 128(2) . .
C14 N3 C17 118(2) . .
C16 N3 C17 113(2) . .
C1 O1 Ca1 145.0(3) . .
C8 O4 Ca1 151.5(3) . 1_455
C8 O5 H5 118(4) . .
C10 O6 Ca1 167.1(5) . .
O6 Ca1 O6 180.0 . 2_766
O6 Ca1 O1 90.29(14) . .
O6 Ca1 O1 89.71(14) 2_766 .
O6 Ca1 O1 89.71(14) . 2_766
O6 Ca1 O1 90.29(14) 2_766 2_766
O1 Ca1 O1 180.00(12) . 2_766
O6 Ca1 O4 90.80(14) . 1_655
O6 Ca1 O4 89.20(14) 2_766 1_655
O1 Ca1 O4 82.70(10) . 1_655
O1 Ca1 O4 97.30(10) 2_766 1_655
O6 Ca1 O4 89.20(14) . 2_666
O6 Ca1 O4 90.80(14) 2_766 2_666
O1 Ca1 O4 97.30(10) . 2_666
O1 Ca1 O4 82.70(10) 2_766 2_666
O4 Ca1 O4 180.0 1_655 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.239(5) .
C1 O2 1.264(5) .
C1 C2 1.508(6) .
C2 C7 1.378(7) .
C2 C3 1.398(6) .
C3 C4 1.392(5) .
C3 N1 1.405(5) .
C4 C5 1.372(6) .
C4 H4 0.9300 .
C5 C6 1.367(6) .
C5 C8 1.493(6) .
C6 C7 1.368(7) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 O4 1.209(5) .
C8 O5 1.299(5) .
C9 O3 1.214(4) .
C9 N1 1.336(5) .
C9 C9 1.546(7) 2_655
C10 N2 1.109(9) .
C10 O6 1.194(8) .
C10 C11 1.706(11) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 N2 1.432(8) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 N2 1.677(10) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 N3 1.29(2) .
C14 O7 1.34(2) .
C14 C15 1.36(2) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 N3 1.374(18) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 N3 1.527(19) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
N1 H1 0.87(4) .
O1 Ca1 2.290(3) .
O4 Ca1 2.337(3) 1_455
O5 H5 0.96(2) .
O6 Ca1 2.249(4) .
Ca1 O6 2.249(4) 2_766
Ca1 O1 2.290(3) 2_766
Ca1 O4 2.337(3) 1_655
Ca1 O4 2.337(3) 2_666
