Hydrogen adsorption in azolium and metalated N-heterocyclic carbene containing MOFs
Capon, Patrick K.; Burgun, Alexandre; Coghlan, Campbell J.; Crees, Rachel S.; Doonan, Christian J.; Sumby, Christopher J.; CrystEngComm 18 (2016) 7003–; doi:10.1039/C6CE01549B

data_7226349
_publ_section_title
;
 Hydrogen adsorption in azolium and metalated N-heterocyclic carbene
 containing MOFs
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7003
_journal_paper_doi               10.1039/C6CE01549B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C75.5 H69.5 Co3 N12.5 O28.5'
_chemical_formula_weight         1784.72
_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
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.37(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.128(5)
_cell_length_b                   14.043(3)
_cell_length_c                   23.412(5)
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      0.76
_cell_volume                     7571(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.923
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       'thin rod'
_exptl_crystal_F_000             3676
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.929
_exptl_transmission_factor_min   0.818
_platon_squeeze_details
;
In order to subtract the contribution from the disordered 
solvent molecules, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 
412, is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to approx 10 DMF molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e). 
;
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9027
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+21.1187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8310
_reflns_number_total             9027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01549b2.cif
_cod_data_source_block           3Co
_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 7226345--7226349.cif.
;
_cod_original_formula_sum        'C75.50 H69.50 Co3 N12.50 O28.50'
_cod_database_code               7226349
_shelx_estimated_absorpt_t_min   0.818
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2014/6
_shelx_res_checksum              725