A dynamic microporous magnet exhibiting room-temperature thermal hysteresis, variable magnetic ordering temperatures and highly selective adsorption for CO2
Liu, Zhong-Yi; Zhao, Hong; Song, Wei-Chao; Wang, Xiu-Guang; Liu, Zheng-Yu; Zhao, Xiao-Jun; Yang, En-Cui; Journal of Materials Chemistry C 7 (2019) 218–; doi:10.1039/C8TC03356K

data_7237471
_publ_section_title
;
 A dynamic microporous magnet exhibiting room-temperature thermal
 hysteresis, variable magnetic ordering temperatures and highly selective
 adsorption for CO2
;
_journal_issue                   2
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              218
_journal_paper_doi               10.1039/C8TC03356K
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety
'0.25(C96 H104 Co20 N88 O60), 4.65(H2 O), 3(O)'
_chemical_formula_sum            'C24 H41.25 Co5 N22 O22.75'
_chemical_formula_weight         1296.69
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-21 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.630(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0069(18)
_cell_length_b                   13.8971(8)
_cell_length_c                   16.1662(12)
_cell_measurement_reflns_used    3801
_cell_measurement_temperature    273.00(10)
_cell_measurement_theta_max      29.3490
_cell_measurement_theta_min      3.7830
_cell_volume                     4900.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5479
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -95.00  -59.00   1.0000  169.5050
omega____ theta____ kappa____ phi______ frames
    -      -12.2164 -178.0000    0.0000 36

  2 omega  -77.00    0.00   1.0000  169.5050
omega____ theta____ kappa____ phi______ frames
    -      -12.2164  -38.0000 -120.0000 77

  3 omega  -24.00   30.00   1.0000  169.5050
omega____ theta____ kappa____ phi______ frames
    -      -12.2164   19.0000   60.0000 54

  4 omega   33.00   67.00   1.0000  169.5050
omega____ theta____ kappa____ phi______ frames
    -      -12.2164   19.0000   60.0000 34

  5 omega   41.00   84.00   1.0000  169.5050
omega____ theta____ kappa____ phi______ frames
    -       12.2164  178.0000  -90.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0228830000
_diffrn_orient_matrix_UB_12      -0.0335484000
_diffrn_orient_matrix_UB_13      0.0079149000
_diffrn_orient_matrix_UB_21      -0.0064600000
_diffrn_orient_matrix_UB_22      -0.0097005000
_diffrn_orient_matrix_UB_23      -0.0433182000
_diffrn_orient_matrix_UB_31      0.0222115000
_diffrn_orient_matrix_UB_32      -0.0372419000
_diffrn_orient_matrix_UB_33      0.0041251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11762
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Purple
_exptl_crystal_colour_primary    Purple
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2625
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.670
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0662
_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/[\s^2^(Fo^2^)+(0.0223P)^2^+66.6631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3257
_reflns_number_total             4291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc03356k2.cif
_cod_data_source_block           a150210b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'NONE' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7237471
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Cu'
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.743
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N10) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O9) = Uanis(O9')
Uanis(O11) = Uanis(O11')
3. Others
 Sof(O9')=Sof(H9'A)=Sof(H9'B)=1-FVAR(1)
 Sof(O9)=Sof(H9C)=Sof(H9D)=FVAR(1)
 Sof(O11')=1-FVAR(2)
 Sof(O11)=FVAR(2)
 Fixed Sof: O7(0.5) H7A(0.5) H7B(0.5) O12(0.325) H12A(0.325) H12B(0.325)
 O13(0.5)
4.a Riding coordinates:
 O8(H8A,H8B), O7(H7A,H7B), O10(H10C,H10D), O12(H12A,H12B)
4.b Free rotating group:
 O9(H9C,H9D,O9',H9'A,H9'B)
4.c Rotating group:
 N4(H4A,H4B), N5(H5A,H5B), N10(H10A,H10B)
4.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8)
4.e X=CH2 refined with riding coordinates:
 N9(H9A,H9B)
;
_olex2_submission_special_instructions 'No special instructions were received'