#------------------------------------------------------------------------------
#$Date: 2016-03-05 10:40:05 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177713 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/06/1540683.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_1540683
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  0.0484
_diffrn_reflns_av_unetI/netI     0.0228
_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
'SC to SC after immersing crystals in a solutione of tianthrene'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.572
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.572
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.1372
_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)+(0.2220P)²+9.9000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3916
_refine_ls_wR_factor_ref         0.4001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2494
_reflns_number_total             2689
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5sc04461h2.cif
_cod_data_source_block           1@TAN
_cod_depositor_comments
'Adding full bibliography for 1540680--1540686.cif.'
_cod_original_cell_volume        4028.4(3)
_cod_database_code               1540683
_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'
'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 0.0216(7) Uani 1 4 d S T P
N1 N 0.3898(6) 0.5000 0.8875(6) 0.0291(19) Uani 1 2 d S T P
C1 C 0.3263(8) 0.5000 0.8252(8) 0.048(3) Uani 1 2 d S T P
S1 S 0.2372(3) 0.5000 0.7416(3) 0.162(4) Uani 1 2 d S T P
N2 N 0.5000 0.6037(4) 1.0000 0.0321(19) Uani 1 2 d S T P
N3 N 0.6069(5) 0.5000 0.8955(5) 0.0225(17) Uani 1 2 d S T P
C2 C 0.4914(6) 0.6383(4) 0.9189(6) 0.0446(19) Uani 1 1 d . . .
H2B H 0.4854 0.6158 0.8597 0.054 Uiso 1 1 calc R U .
C3 C 0.4907(6) 0.7035(4) 0.9165(6) 0.047(2) Uani 1 1 d . . .
H3A H 0.4838 0.7253 0.8567 0.056 Uiso 1 1 calc R U .
C4 C 0.5000 0.7380(5) 1.0000 0.038(2) Uani 1 2 d S T P
C5 C 0.5000 0.8062(6) 1.0000 0.046(3) Uani 1 2 d S T P
C6 C 0.5000 0.8650(5) 1.0000 0.040(3) Uani 1 2 d S T P
C7 C 0.5000 0.9331(5) 1.0000 0.038(3) Uani 1 2 d S T P
C8 C 0.4595(5) 0.9666(3) 1.0704(5) 0.0372(17) Uani 1 1 d . . .
H8A H 0.4316 0.9438 1.1188 0.045 Uiso 1 1 calc R U .
C9 C 0.7007(8) 0.5000 0.9235(8) 0.050(3) Uani 1 2 d S T P
H9A H 0.7214 0.5000 0.9904 0.060 Uiso 1 2 calc R U P
C10 C 0.7713(8) 0.5000 0.8627(8) 0.067(4) Uani 1 2 d S T P
H10A H 0.8382 0.5000 0.8878 0.081 Uiso 1 2 calc R U P
C11 C 0.7439(7) 0.5000 0.7630(7) 0.036(2) Uani 1 2 d S T P
C12 C 0.6468(10) 0.5000 0.7346(9) 0.075(5) Uani 1 2 d S T P
H12A H 0.6229 0.5000 0.6684 0.089 Uiso 1 2 calc R U P
C13 C 0.5822(8) 0.5000 0.8037(7) 0.058(4) Uani 1 2 d S T P
H13A H 0.5146 0.5000 0.7815 0.069 Uiso 1 2 calc R U P
C14 C 0.8129(8) 0.5000 0.6998(7) 0.045(3) Uani 1 2 d S T P
C15 C 0.8696(8) 0.5000 0.6378(8) 0.053(3) Uani 1 2 d S T P
C16 C 0.9359(8) 0.5000 0.5694(7) 0.051(3) Uani 1 2 d S T P
C17 C 0.9034(9) 0.5000 0.4748(9) 0.159(13) Uani 1 2 d S T P
H17A H 0.8353 0.5000 0.4546 0.191 Uiso 1 2 calc R U P
C18 C 0.9686(11) 0.5000 0.4061(10) 0.161(13) Uani 1 2 d S T P
H18A H 0.9437 0.5000 0.3402 0.193 Uiso 1 2 calc R U P
C11S C 1.0000 0.0000 1.5000 0.129(11) Uiso 1 4 d S . P
C7S C 0.9870 0.0932 1.4043 0.208 Uiso 1 1 d . . .
C8S C 1.0704 0.0304 1.4579 0.255 Uiso 1 1 d . . .
C9S C 0.9023 0.0991 1.4525 0.205 Uiso 1 1 d . . .
S2S S 0.8191(5) 0.1541(3) 1.4024(4) 0.0839(19) Uani 0.5 1 d . . P
S3S S 1.0461(10) 0.1489(4) 1.3357(5) 0.146(4) Uani 0.5 1 d . . P
C1S C 1.0107(15) 0.3340(9) 1.3617(18) 0.136(12) Uiso 0.5 1 d G . P
H1SA H 1.0514 0.3696 1.3520 0.163 Uiso 0.5 1 calc R U P
C2S C 0.9197(16) 0.3441(7) 1.3912(16) 0.135(12) Uiso 0.5 1 d G . P
H2SA H 0.8981 0.3865 1.4017 0.162 Uiso 0.5 1 calc R U P
C3S C 0.8601(12) 0.2921(9) 1.4053(15) 0.094(7) Uiso 0.5 1 d G . P
H3SA H 0.7979 0.2990 1.4254 0.112 Uiso 0.5 1 calc R U P
C4S C 0.8916(14) 0.2300(8) 1.3899(15) 0.116(9) Uiso 0.5 1 d G . P
C5S C 0.9826(15) 0.2199(8) 1.3604(15) 0.099(8) Uiso 0.5 1 d G . P
C6S C 1.0422(12) 0.2719(11) 1.3463(16) 0.130(11) Uiso 0.5 1 d G . P
H6SA H 1.1044 0.2650 1.3261 0.156 Uiso 0.5 1 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(2) . 5_667
N1 Co1 N2 90.000(1) 5_667 5_667
N1 Co1 N2 90.000(1) . .
N1 Co1 N2 90.000(2) 5_667 .
N2 Co1 N2 180.0 5_667 .
N1 Co1 N3 88.9(3) . .
N1 Co1 N3 91.1(3) 5_667 .
N2 Co1 N3 90.0 5_667 .
N2 Co1 N3 90.000(2) . .
N1 Co1 N3 91.1(3) . 5_667
N1 Co1 N3 88.9(3) 5_667 5_667
N2 Co1 N3 90.000(2) 5_667 5_667
N2 Co1 N3 90.000(1) . 5_667
N3 Co1 N3 180.0 . 5_667
C1 N1 Co1 178.7(8) . .
N1 C1 S1 178.6(10) . .
C2 N2 C2 115.3(9) 2_657 .
C2 N2 Co1 122.4(4) 2_657 .
C2 N2 Co1 122.4(4) . .
C13 N3 C9 115.6(9) . .
C13 N3 Co1 123.1(6) . .
C9 N3 Co1 121.2(6) . .
N2 C2 C3 123.8(7) . .
C2 C3 C4 120.2(7) . .
C3 C4 C3 116.8(9) 2_657 .
C3 C4 C5 121.6(5) 2_657 .
C3 C4 C5 121.6(5) . .
C6 C5 C4 180.0 . .
C5 C6 C7 180.0 . .
C8 C7 C8 119.5(9) 2_657 .
C8 C7 C6 120.2(5) 2_657 .
C8 C7 C6 120.2(5) . .
C7 C8 C8 120.2(5) . 6_575
N3 C9 C10 124.4(10) . .
C9 C10 C11 119.7(10) . .
C12 C11 C14 123.2(10) . .
C12 C11 C10 115.6(10) . .
C14 C11 C10 121.2(9) . .
C11 C12 C13 119.3(11) . .
N3 C13 C12 125.4(10) . .
C15 C14 C11 175.6(12) . .
C14 C15 C16 178.6(12) . .
C18 C16 C17 117.3(11) 5_766 .
C18 C16 C15 122.3(11) 5_766 .
C17 C16 C15 120.4(11) . .
C18 C17 C16 120.9(12) . .
C16 C18 C17 121.8(12) 5_766 .
C8S C11S C8S 124.4 5_758 6
C8S C11S C8S 55.6 5_758 2_758
C8S C11S C8S 180.0 6 2_758
C8S C11S C8S 180.0 5_758 .
C8S C11S C8S 55.6 6 .
C8S C11S C8S 124.4 2_758 .
C9S C7S S3S 131.5(4) . .
C9S C7S C8S 112.0 . .
S3S C7S C8S 112.3(4) . .
C8S C8S C11S 62.2 6 .
C8S C8S C7S 135.1 6 .
C11S C8S C7S 93.6 . .
C8S C8S C9S 138.4 6 2_758
C11S C8S C9S 99.0 . 2_758
C7S C8S C9S 78.7 . 2_758
C7S C9S S2S 114.2(2) . .
C7S C9S C8S 98.1 . 2_758
S2S C9S C8S 147.1(2) . 2_758
C9S S2S C4S 105.0(7) . .
C7S S3S C5S 99.6(9) . .
C2S C1S C6S 120.0 . .
C1S C2S C3S 120.0 . .
C4S C3S C2S 120.0 . .
C5S C4S C3S 120.0 . .
C5S C4S S2S 114.3(12) . .
C3S C4S S2S 125.6(12) . .
C4S C5S C6S 120.0 . .
C4S C5S S3S 132.2(13) . .
C6S C5S S3S 107.7(13) . .
C5S C6S C1S 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.061(8) .
Co1 N1 2.061(8) 5_667
Co1 N2 2.160(8) 5_667
Co1 N2 2.160(8) .
Co1 N3 2.211(7) .
Co1 N3 2.211(7) 5_667
N1 C1 1.163(14) .
C1 S1 1.599(11) .
N2 C2 1.342(9) 2_657
N2 C2 1.343(9) .
N3 C13 1.296(13) .
N3 C9 1.310(13) .
C2 C3 1.360(11) .
C3 C4 1.371(10) .
C4 C3 1.371(10) 2_657
C4 C5 1.419(16) .
C5 C6 1.224(16) .
C6 C7 1.418(15) .
C7 C8 1.385(9) 2_657
C7 C8 1.385(9) .
C8 C8 1.393(15) 6_575
C9 C10 1.374(16) .
C10 C11 1.409(15) .
C11 C12 1.354(17) .
C11 C14 1.384(15) .
C12 C13 1.400(17) .
C14 C15 1.243(16) .
C15 C16 1.408(15) .
C16 C18 1.324(19) 5_766
C16 C17 1.353(18) .
C17 C18 1.40(2) .
C18 C16 1.324(19) 5_766
C11S C8S 1.3574 5_758
C11S C8S 1.3574 6
C11S C8S 1.3574 2_758
C11S C8S 1.3574 .
C7S C9S 1.4297 .
C7S S3S 1.771(11) .
C7S C8S 1.8440 .
C8S C8S 1.2668 6
C8S C9S 1.9131 2_758
C9S S2S 1.714(5) .
C9S C8S 1.9132 2_758
S2S C4S 1.891(16) .
S3S C5S 1.776(17) .
C1S C2S 1.3900 .
C1S C6S 1.3900 .
C2S C3S 1.3900 .
C3S C4S 1.3900 .
C4S C5S 1.3900 .
C5S C6S 1.3900 .
