#------------------------------------------------------------------------------
#$Date: 2016-03-05 10:40:05 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177713 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/06/1540682.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_1540682
loop_
_publ_author_name
'Vallejo, Julia'
'Fortea-Pérez, Francisco R.'
'Pardo, Emilio'
'Benmansour, Samia'
'Castro, Isabel'
'Krzystek, J.'
'Armentano, Donatella'
'Cano, Joan'
_publ_section_title
;
 Guest-dependent single-ion magnet behaviour in a cobalt(ii)
 metal--organic framework
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2286
_journal_paper_doi               10.1039/C5SC04461H
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C94 H72 Co N6 O4 S10'
_chemical_formula_weight         1729.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-30 deposited with the CCDC.
2015-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.987(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8432(9)
_cell_length_b                   20.8218(9)
_cell_length_c                   14.0803(6)
_cell_measurement_reflns_used    4532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.8
_cell_measurement_theta_min      3.2
_cell_volume                     4028.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.717
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_laue_measured_fraction_full 0.717
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34324
_diffrn_reflns_point_group_measured_fraction_full 0.717
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.412
_diffrn_reflns_theta_min         1.457
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       CUBIC/PRISM
_exptl_crystal_F_000             1794
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Single-crystal to single-crystal immersing crystals in a solution of tiantrene'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0697
_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)+(0.1327P)²+9.6945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2472
_reflns_number_total             2689
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5sc04461h2.cif
_cod_data_source_block           1@tan_sq
_cod_depositor_comments
'Adding full bibliography for 1540680--1540686.cif.'
_cod_original_cell_volume        4028.4(3)
_cod_database_code               1540682
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.5000 0.5000 1.0000 0.0217(4) Uani 1 4 d S T P
N1 N 0.3899(3) 0.5000 0.8879(3) 0.0313(10) Uani 1 2 d S T P
C1 C 0.3252(4) 0.5000 0.8259(4) 0.0536(17) Uani 1 2 d S T P
S1 S 0.23755(17) 0.5000 0.74200(17) 0.1588(18) Uani 1 2 d S T P
N2 N 0.5000 0.60430(19) 1.0000 0.0328(10) Uani 1 2 d S T P
N3 N 0.6061(3) 0.5000 0.8948(3) 0.0248(9) Uani 1 2 d S T P
C2 C 0.4895(3) 0.63815(19) 0.9185(3) 0.0448(10) Uani 1 1 d . . .
H2B H 0.4805 0.6154 0.8596 0.054 Uiso 1 1 calc R U .
C3 C 0.4910(3) 0.7034(2) 0.9157(3) 0.0492(11) Uani 1 1 d . . .
H3A H 0.4859 0.7251 0.8560 0.059 Uiso 1 1 calc R U .
C4 C 0.5000 0.7380(2) 1.0000 0.0363(13) Uani 1 2 d S T P
C5 C 0.5000 0.8071(3) 1.0000 0.0421(14) Uani 1 2 d S T P
C6 C 0.5000 0.8641(3) 1.0000 0.0418(14) Uani 1 2 d S T P
C7 C 0.5000 0.9337(2) 1.0000 0.0376(13) Uani 1 2 d S T P
C8 C 0.4583(3) 0.96712(18) 1.0697(3) 0.0362(9) Uani 1 1 d . . .
H8A H 0.4296 0.9444 1.1176 0.043 Uiso 1 1 calc R U .
C9 C 0.7017(4) 0.5000 0.9227(4) 0.0544(18) Uani 1 2 d S T P
H9A H 0.7232 0.5000 0.9894 0.065 Uiso 1 2 calc R U P
C10 C 0.7700(4) 0.5000 0.8610(4) 0.065(2) Uani 1 2 d S T P
H10A H 0.8372 0.5000 0.8851 0.078 Uiso 1 2 calc R U P
C11 C 0.7426(4) 0.5000 0.7645(4) 0.0397(13) Uani 1 2 d S T P
C12 C 0.6484(5) 0.5000 0.7369(4) 0.075(2) Uani 1 2 d S T P
H12A H 0.6255 0.5000 0.6704 0.089 Uiso 1 2 calc R U P
C13 C 0.5816(4) 0.5000 0.8033(4) 0.060(2) Uani 1 2 d S T P
H13A H 0.5142 0.5000 0.7799 0.072 Uiso 1 2 calc R U P
C14 C 0.8127(4) 0.5000 0.6981(4) 0.0505(16) Uani 1 2 d S T P
C15 C 0.8688(4) 0.5000 0.6380(4) 0.0545(17) Uani 1 2 d S T P
C16 C 0.9349(4) 0.5000 0.5680(4) 0.0544(17) Uani 1 2 d S T P
C17 C 0.9041(5) 0.5000 0.4750(5) 0.147(6) Uani 1 2 d S T P
H17A H 0.8361 0.5000 0.4545 0.176 Uiso 1 2 calc R U P
C18 C 0.9678(5) 0.5000 0.4077(5) 0.161(7) Uani 1 2 d S T P
H18A H 0.9426 0.5000 0.3419 0.193 Uiso 1 2 calc R U 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'
S S 0.1246 0.1234 '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'
Co Co 0.3494 0.9721 '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 Co1 N1 180.0 5_667 .
N1 Co1 N2 90.000(1) 5_667 .
N1 Co1 N2 90.000(1) . .
N1 Co1 N2 90.000(1) 5_667 5_667
N1 Co1 N2 90.000(1) . 5_667
N2 Co1 N2 180.0 . 5_667
N1 Co1 N3 91.34(14) 5_667 .
N1 Co1 N3 88.66(14) . .
N2 Co1 N3 90.000(1) . .
N2 Co1 N3 90.0 5_667 .
N1 Co1 N3 88.66(14) 5_667 5_667
N1 Co1 N3 91.34(14) . 5_667
N2 Co1 N3 90.0 . 5_667
N2 Co1 N3 90.000(1) 5_667 5_667
N3 Co1 N3 180.0 . 5_667
C1 N1 Co1 178.1(4) . .
N1 C1 S1 180.0(5) . .
C2 N2 C2 116.5(4) 2_657 .
C2 N2 Co1 121.8(2) 2_657 .
C2 N2 Co1 121.8(2) . .
C13 N3 C9 115.1(4) . .
C13 N3 Co1 123.6(3) . .
C9 N3 Co1 121.3(3) . .
N2 C2 C3 123.4(4) . .
C2 C3 C4 119.8(4) . .
C3 C4 C3 117.1(5) 2_657 .
C3 C4 C5 121.4(2) 2_657 .
C3 C4 C5 121.5(2) . .
C6 C5 C4 180.0 . .
C5 C6 C7 180.0 . .
C8 C7 C8 119.7(5) 2_657 .
C8 C7 C6 120.2(2) 2_657 .
C8 C7 C6 120.2(2) . .
C8 C8 C7 120.2(2) 6_575 .
N3 C9 C10 123.7(5) . .
C9 C10 C11 120.3(6) . .
C12 C11 C10 116.2(5) . .
C12 C11 C14 122.3(5) . .
C10 C11 C14 121.5(5) . .
C11 C12 C13 121.1(6) . .
N3 C13 C12 123.7(5) . .
C15 C14 C11 176.9(6) . .
C14 C15 C16 179.7(6) . .
C17 C16 C18 116.1(6) . 5_766
C17 C16 C15 121.8(6) . .
C18 C16 C15 122.1(6) 5_766 .
C16 C17 C18 121.7(6) . .
C16 C18 C17 122.2(6) 5_766 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.056(4) 5_667
Co1 N1 2.056(4) .
Co1 N2 2.172(4) .
Co1 N2 2.172(4) 5_667
Co1 N3 2.209(4) .
Co1 N3 2.209(4) 5_667
N1 C1 1.173(7) .
C1 S1 1.587(6) .
N2 C2 1.339(4) 2_657
N2 C2 1.339(4) .
N3 C13 1.292(7) .
N3 C9 1.334(7) .
C2 C3 1.359(6) .
C3 C4 1.381(5) .
C4 C3 1.381(5) 2_657
C4 C5 1.439(8) .
C5 C6 1.187(8) .
C6 C7 1.449(8) .
C7 C8 1.386(5) 2_657
C7 C8 1.386(5) .
C8 C8 1.369(8) 6_575
C9 C10 1.360(8) .
C10 C11 1.366(8) .
C11 C12 1.314(9) .
C11 C14 1.428(8) .
C12 C13 1.393(9) .
C14 C15 1.215(8) .
C15 C16 1.424(8) .
C16 C17 1.327(9) .
C16 C18 1.349(10) 5_766
C17 C18 1.371(11) .
C18 C16 1.349(10) 5_766
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.003 0.255 0.402 2677 895 ' '
