Structural stabilization of a metal-organic framework for gas sorption investigation.
Gao, Qiang; Zhao, Xiao-Lin; Chang, Ze; Xu, Jian; Bu, Xian-He; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6830–6833; doi:10.1039/c6dt00640j

data_7038805
_publ_section_title
;
 Structural stabilization of a metal-organic framework for gas sorption
 investigation.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6830
_journal_page_last               6833
_journal_paper_doi               10.1039/c6dt00640j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
Co3(O)(C9H6N3O2)3(C18H12N6)(NO3)(H2O)(C2H6O)7(C3H7NO)8
_chemical_formula_sum            'C45 H30 Co3 N15 O7'
_chemical_formula_weight         1069.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1kgg3l
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-03-16 deposited with the CCDC.
2016-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.679(2)
_cell_length_b                   16.679(2)
_cell_length_c                   19.050(4)
_cell_measurement_reflns_used    8860
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.0196
_cell_measurement_theta_min      1.4081
_cell_volume                     4589.5(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn70 (4x4 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37425
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.976
_diffrn_reflns_theta_min         1.410
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Higashi,T.(1995).
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    0.774
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
In the final refinement, the contributions of disordered 
counter ions and solvent to the structure factors in 
Co-MOF1-tpt were removed with the SQUEEZE program 
and the crystal structure was then further refined with new 
hkl file generated by the SQUEEZE calculation. Based on
the SQUEEZE calculation results, IR, TG analysis,one NO3-,
one water moleculer, seven EtOH and eight DMF moleculers 
were added directly to the final molecular formula.
;
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2862
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0912P)^2^+3.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1691
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2517
_reflns_number_total             2862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00640j2.cif
_cod_data_source_block           Co_MOF1_tpt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038805.cif.
;
_cod_original_cell_volume        4589.5(15)
_cod_database_code               7038805
_shelxl_version_number           2014-3
_shelx_res_checksum              92835