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_7226347
_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            'C72.5 H60.5 Mn3 N11.5 O26.5'
_chemical_formula_weight         1681.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                63.88(3)
_cell_angle_beta                 79.87(3)
_cell_angle_gamma                89.57(3)
_cell_formula_units_Z            1
_cell_length_a                   11.014(2)
_cell_length_b                   13.053(3)
_cell_length_c                   14.145(3)
_cell_measurement_reflns_used    7871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      0.76
_cell_volume                     1791.8(8)
_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 0.925
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30395
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_min         1.634
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'light brown/orange'
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             863
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.930
_exptl_transmission_factor_min   0.847
_platon_squeeze_details
;
In order to subtract the contribution from the disordered 
solvent molecules and anions not located in the 
difference map, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 
129, is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to the 2 NO3 anions and approx 1.5 DMF 
molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e; one NO3- anion would
give 32 e). 
;
_refine_diff_density_max         2.915
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1502P)^2^+0.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5359
_reflns_number_total             7854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01549b2.cif
_cod_data_source_block           5Mn
_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        'C72.50 H60.50 Mn3 N11.50 O26.50'
_cod_database_code               7226347
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2014/6
_shelx_res_checksum              47603