Guest-induced reversible crystal-to-amorphous-to-crystal transformation in a Co(ii)-based metal‒organic framework
Tan, Huiling; Chen, Qibin; Sheng, Yujie; Li, Xiaoxiao; Liu, Honglai; CrystEngComm 20 (2018) 6828–; doi:10.1039/C8CE01324A

data_7231602
_publ_section_title
;
 Guest-induced reversible crystal-to-amorphous-to-crystal transformation
 in a Co(ii)-based metal--organic framework
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6828
_journal_paper_doi               10.1039/C8CE01324A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '0.5(C58 H46 Co2 N4 O8), 3.5(H2 O)'
_chemical_formula_sum            'C29 H30 Co N2 O7.5'
_chemical_formula_weight         585.48
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.308(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.715(7)
_cell_length_b                   23.065(9)
_cell_length_c                   9.764(4)
_cell_measurement_reflns_used    1867
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.63
_cell_measurement_theta_min      2.36
_cell_volume                     3360(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13526
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.814
_diffrn_reflns_theta_min         2.819
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0707 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.8711. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3892
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0606
_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^)+(0.1185P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2018
_reflns_number_total             3892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01324a2.cif
_cod_data_source_block           mo_dm17196_0m
_cod_depositor_comments          'Adding full bibliography for 7231602.cif.'
_cod_original_formula_sum        'C29 H30 Co N2 O7.50'
_cod_database_code               7231602
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5) O5(0.25) H5A(0.25) H5B(0.25)
4.a Free rotating group:
 O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B)
4.b Rotating group:
 O2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14)
;
_shelx_res_checksum              75929
_shelx_fab_checksum              59676
_olex2_submission_special_instructions 'No special instructions were received'